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CN116179883B - A method for preparing nano NbB2 particle reinforced NiAl alloy - Google Patents

A method for preparing nano NbB2 particle reinforced NiAl alloy Download PDF

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CN116179883B
CN116179883B CN202211692266.8A CN202211692266A CN116179883B CN 116179883 B CN116179883 B CN 116179883B CN 202211692266 A CN202211692266 A CN 202211692266A CN 116179883 B CN116179883 B CN 116179883B
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CN116179883A (en
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杨宏宇
钟鑫淼
董柏欣
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Jilin University
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/10Alloys containing non-metals
    • C22C1/1036Alloys containing non-metals starting from a melt
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C19/00Alloys based on nickel or cobalt
    • C22C19/03Alloys based on nickel or cobalt based on nickel
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C32/00Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ
    • C22C32/0047Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents
    • C22C32/0073Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
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Abstract

The invention discloses a preparation method of nano NbB 2 particle reinforced NiAl alloy, which comprises the following steps: 1. preparing nickel-coated NbB 2 nano particles; 2. placing a NiAl alloy raw material into a water-cooled copper crucible in a smelting chamber of vacuum smelting equipment, and respectively placing nickel-coated NbB 2 nano particles and Al powder into a feed port of the vacuum smelting equipment; wherein the vacuum degree in the smelting chamber is kept between 5Pa and 20Pa; 3. filling inert gas into the smelting chamber to keep the pressure of the smelting chamber at 10000 Pa-20000 Pa; heating the smelting chamber, and gradually increasing the heating power until the NiAl alloy is completely melted to obtain a NiAl alloy melt; 4. adding nickel-coated NbB 2 nano particles at a feed port into a NiAl alloy melt in a water-cooled copper crucible; after fully dispersing NbB 2 nano particles in the NiAl melt by electromagnetic induction stirring, adding Al powder to obtain an enhanced NiAl alloy melt; 5. casting the reinforced NiAl alloy melt with a grinder in a smelting chamber; and after casting and cooling, obtaining the nano NbB 2 particle reinforced NiAl alloy.

Description

一种纳米NbB2颗粒增强NiAl合金制备方法A method for preparing nano NbB2 particle reinforced NiAl alloy

技术领域Technical Field

本发明属于纳米颗粒强化高温镍铝基合金技术领域,特别涉及一种纳米NbB2颗粒增强NiAl合金制备方法。The invention belongs to the technical field of nano-particle reinforced high-temperature nickel-aluminum-based alloys, and particularly relates to a method for preparing a nano- NbB2 particle reinforced NiAl alloy.

背景技术Background technique

随着我国航空航天工业升级改造,对于先进高性能材料性能的需求不断提高,急需开发高性能高温合金及其强化手段。近期研究表明,纳米颗粒尤其是纳米陶瓷可高效强化高温合金材料,但是纳米颗粒由于较大的比表面积造成极易表面吸附和颗粒彼此团聚,因此,如何解决纳米颗粒的团聚问题,如何解决纳米颗粒加入到熔体后的分散问题将是强化高温合金材料的重要问题,具有显著意义及实际应用价值。With the upgrading and transformation of my country's aerospace industry, the demand for advanced high-performance materials is constantly increasing, and there is an urgent need to develop high-performance high-temperature alloys and their strengthening methods. Recent studies have shown that nanoparticles, especially nanoceramics, can effectively strengthen high-temperature alloy materials. However, due to the large specific surface area, nanoparticles are very easy to adsorb on the surface and agglomerate with each other. Therefore, how to solve the agglomeration problem of nanoparticles and how to solve the dispersion problem of nanoparticles after adding them to the melt will be an important issue in strengthening high-temperature alloy materials, which has significant significance and practical application value.

发明内容Summary of the invention

本发明的目的是提供一种纳米NbB2颗粒增强NiAl合金制备方法,其能够改善NbB2陶瓷颗粒在NiAl合金中团聚现象,并且使镍包覆的NbB2陶瓷颗粒与NiAl合金的界面结合得到提高。The purpose of the present invention is to provide a method for preparing a nano NbB2 particle reinforced NiAl alloy, which can improve the agglomeration phenomenon of NbB2 ceramic particles in the NiAl alloy and improve the interface bonding between the nickel-coated NbB2 ceramic particles and the NiAl alloy.

本发明提供的技术方案为:The technical solution provided by the present invention is:

一种纳米NbB2颗粒增强NiAl合金制备方法,包括如下步骤:A method for preparing a nano NbB2 particle reinforced NiAl alloy comprises the following steps:

步骤一、制备镍包覆NbB2纳米颗粒;Step 1, preparing nickel-coated NbB2 nanoparticles;

步骤二、将NiAl合金原料放入真空熔炼设备熔炼室内的水冷铜坩埚中,将所述镍包覆NbB2纳米颗粒和Al粉分别放入真空熔炼设备熔炼室的投料口;Step 2: Place the NiAl alloy raw material into a water-cooled copper crucible in the melting chamber of the vacuum melting equipment, and place the nickel-coated NbB2 nanoparticles and Al powder into the feeding port of the melting chamber of the vacuum melting equipment respectively;

其中,熔炼室内的真空度保持在5Pa~20Pa;Among them, the vacuum degree in the smelting chamber is maintained at 5Pa~20Pa;

步骤三、向所述熔炼室内充入惰性气体,使所述熔炼室的压力保持在10000Pa~20000Pa;熔炼室开始加热,并且逐渐增大加热功率,直到NiAl合金全部熔化,得到NiAl合金熔体;Step 3, filling the smelting chamber with inert gas to keep the pressure of the smelting chamber at 10000Pa-20000Pa; starting heating the smelting chamber and gradually increasing the heating power until the NiAl alloy is completely melted to obtain a NiAl alloy melt;

步骤四、将投料口处的镍包覆NbB2纳米颗粒加入到水冷铜坩埚中NiAl合金熔体内;通过电磁感应搅拌使得NbB2纳米颗粒在NiAl熔体中充分分散后,加入Al粉,得到增强的NiAl合金熔体;Step 4: adding the nickel-coated NbB2 nanoparticles at the feeding port into the NiAl alloy melt in the water-cooled copper crucible; after the NbB2 nanoparticles are fully dispersed in the NiAl melt by electromagnetic induction stirring, Al powder is added to obtain an enhanced NiAl alloy melt;

其中,NbB2纳米颗粒的质量占增强的NiAl合金熔体总质量的0.05~0.30wt.%;Wherein, the mass of NbB2 nanoparticles accounts for 0.05-0.30wt.% of the total mass of the enhanced NiAl alloy melt;

步骤五、在所述熔炼室内,利用磨具浇铸增强的NiAl合金熔体;浇铸完成并冷却后,得到所述纳米NbB2颗粒增强NiAl合金。Step 5: In the smelting chamber, the reinforced NiAl alloy melt is cast using a mold; after the casting is completed and cooled, the nano NbB2 particle reinforced NiAl alloy is obtained.

优选的是,在所述步骤一中,制备镍包覆NbB2纳米颗粒,包括如下步骤:Preferably, in step 1, preparing nickel-coated NbB2 nanoparticles comprises the following steps:

步骤1、将镍粉与NbB2粉体混合,并放入球磨机内均匀化处理,得到混合粉体;Step 1, mixing nickel powder and NbB2 powder, and putting them into a ball mill for homogenization to obtain a mixed powder;

其中,镍粉的粒径为20微米~200微米,NbB2粉体粒径为10微米~100微米;所述混合粉体中,镍粉的占比为20~50wt%;The particle size of the nickel powder is 20 microns to 200 microns, and the particle size of the NbB2 powder is 10 microns to 100 microns; in the mixed powder, the nickel powder accounts for 20 to 50 wt%;

步骤2、在真空反应室中充入惰性气体,利用高频直流电源产生稳定的惰性气体混合热等离子体;将所述混合粉体送入所述真空反应室,经过所述热等离子体后反应后,经快速冷却,得到镍包覆的NbB2粉体;Step 2, filling the vacuum reaction chamber with an inert gas, and using a high-frequency DC power supply to generate a stable inert gas mixed thermal plasma; sending the mixed powder into the vacuum reaction chamber, after the thermal plasma post-reaction, and then rapidly cooling, to obtain nickel-coated NbB2 powder;

步骤3、在所述镍包覆的NbB2粉体中筛选出600纳米以下的颗粒,即为所述镍包覆NbB2纳米颗粒。Step 3: Screen out particles with a size of less than 600 nanometers from the nickel-coated NbB2 powder, namely the nickel-coated NbB2 nanoparticles.

优选的是,在所述步骤2中,充入惰性气体的真空反应室的气压处于0.01MPa~0.03MPa。Preferably, in step 2, the pressure of the vacuum reaction chamber filled with inert gas is between 0.01 MPa and 0.03 MPa.

优选的是,在所述步骤2中,以3米/秒~20米/秒的速度将所述混合粉体送入所述真空反应室。Preferably, in step 2, the mixed powder is fed into the vacuum reaction chamber at a speed of 3 m/s to 20 m/s.

优选的是,在所述步骤三中制备NiAl合金熔体过程中,加热功率每次提升3kW~7kW并保持5~8分钟。Preferably, during the preparation of the NiAl alloy melt in step 3, the heating power is increased by 3 kW to 7 kW each time and maintained for 5 to 8 minutes.

优选的是,在所述步骤四中,NbB2纳米颗粒在NiAl熔体中充分分散40秒~80秒后,加入Al粉。Preferably, in the step 4, Al powder is added after the NbB2 nanoparticles are fully dispersed in the NiAl melt for 40 seconds to 80 seconds.

优选的是,在所述步骤四中,加入Al粉3分钟~7分钟后,进行浇铸。Preferably, in the step 4, casting is performed 3 to 7 minutes after the Al powder is added.

优选的是,在所述步骤五中,浇铸过程中逐渐降低熔炼设备的功率至0。Preferably, in step five, the power of the smelting equipment is gradually reduced to 0 during the casting process.

优选的是,在所述步骤五中,采用石墨模具进行浇铸。Preferably, in step five, a graphite mold is used for casting.

优选的是,在所述步骤五中,在进行浇铸前,还包括将所述模具提前放在真空熔炼室中进行预热。Preferably, in the step five, before casting, the mold is placed in a vacuum melting chamber for preheating.

本发明的有益效果是:The beneficial effects of the present invention are:

本发明提供的纳米NbB2颗粒增强NiAl合金制备方法,其能够改善NbB2陶瓷颗粒在NiAl合金中团聚现象,并且使镍包覆的NbB2陶瓷颗粒与NiAl合金的界面结合得到提高。该制备方法简单易控制和自动化,具有着重要的实际应用价值。The method for preparing a nano NbB2 particle reinforced NiAl alloy provided by the present invention can improve the agglomeration phenomenon of NbB2 ceramic particles in the NiAl alloy and improve the interface bonding between the nickel-coated NbB2 ceramic particles and the NiAl alloy. The method is simple, easy to control and automated, and has important practical application value.

附图说明BRIEF DESCRIPTION OF THE DRAWINGS

图1为本发明对比例1的NiAl合金显微组织。FIG. 1 is a NiAl alloy microstructure of Comparative Example 1 of the present invention.

图2为本发明实施例1的NiAl-0.05wt.%合金显微组织。FIG. 2 is the microstructure of the NiAl-0.05wt.% alloy of Example 1 of the present invention.

图3为本发明实施例1的X射线衍射相分析。FIG3 is an X-ray diffraction phase analysis of Example 1 of the present invention.

图4为本发明实施例1的镍包覆NbB2纳米颗粒组织形貌图。FIG. 4 is a microstructure morphology of nickel-coated NbB 2 nanoparticles according to Example 1 of the present invention.

图5为本发明实施例2的NiAl-0.15wt.%合金显微组织。FIG. 5 is the microstructure of the NiAl-0.15wt.% alloy of Example 2 of the present invention.

图6为本发明实施例2的X射线衍射相分析。FIG6 is an X-ray diffraction phase analysis of Example 2 of the present invention.

图7为本发明实施例2的镍包覆NbB2纳米颗粒组织形貌图。FIG. 7 is a microstructure morphology of nickel-coated NbB 2 nanoparticles according to Example 2 of the present invention.

图8为本发明实施例3的NiAl-0.3wt.%合金显微组织。FIG. 8 is the microstructure of the NiAl-0.3wt.% alloy of Example 3 of the present invention.

图9为本发明实施例3的X射线衍射相分析。FIG. 9 is an X-ray diffraction phase analysis of Example 3 of the present invention.

图10为本发明实施例3的镍包覆NbB2纳米颗粒组织形貌图。FIG. 10 is a microstructure morphology of nickel-coated NbB 2 nanoparticles according to Example 3 of the present invention.

具体实施方式Detailed ways

下面结合附图对本发明做进一步的详细说明,以令本领域技术人员参照说明书文字能够据以实施。The present invention will be further described in detail below in conjunction with the accompanying drawings so that those skilled in the art can implement the invention with reference to the description.

本发明提供了一种纳米NbB2颗粒增强NiAl合金制备方法,具体制备过程如下,制备过程在高频感应等离子体制备纳米粉体装置和真空熔炼设备熔炼室中进行。The invention provides a method for preparing a nano NbB2 particle reinforced NiAl alloy. The specific preparation process is as follows. The preparation process is carried out in a high-frequency induction plasma nano powder preparation device and a vacuum melting equipment melting chamber.

(1)高频感应等离子体制备镍包覆NbB2纳米颗粒;(1) Preparation of nickel-coated NbB2 nanoparticles by high-frequency induction plasma;

(1a)微米镍粉和微米NbB2粉体混合物配置和均匀混合:(1a) Preparation and uniform mixing of micron nickel powder and micron NbB2 powder mixture:

配置混合粉体,成分为:50wt%~80wt%微米NbB2粉,NbB2粉体尺寸为10~100微米,纯度99.5wt%;20wt%~50wt%微米镍粉,镍粉体尺寸为20-200微米,纯度99.5wt%;将配好的混合粉体放入球磨机内以10~60r/min的速度进行均匀化处理,混合30-90分钟;将球磨后的粉料取出,待用。Prepare a mixed powder, the ingredients of which are: 50wt% to 80wt% micron NbB2 powder , the size of which is 10 to 100 microns, and the purity of which is 99.5wt%; 20wt% to 50wt% micron nickel powder, the size of which is 20-200 microns, and the purity of which is 99.5wt%; put the prepared mixed powder into a ball mill for homogenization treatment at a speed of 10 to 60 r/min, and mix for 30 to 90 minutes; take out the ball-milled powder for standby use.

(1b)微米镍粉和微米NbB2粉体混合物经高频感应等离子体制备镍包覆NbB2纳米颗粒:(1b) Preparation of nickel-coated NbB2 nanoparticles by high-frequency induction plasma from a mixture of micron nickel powder and micron NbB2 powder:

首先使充入惰性气体的真空反应室的气压处于0.01~0.03MPa,利用高频电源和直流电源产生稳定的惰性混合气体热等离子体。随后以3~20米/秒的速度将微米镍粉和微米NbB2粉体混合物送进反应室,高能量密度热等离子体作用于混合粉体时,产生等离子体,该等离子体在扩散过程中,不断与惰性气体原子发生激烈的碰撞,然后利用冷却装置迅速冷却,自发成核并凝聚生长成超微粒团簇,团簇形成后,通过气体对流作用而迅速离开过饱和区,最后沉积在粒子收集装置的器壁,由于NbB2熔点高而先形核凝固,镍熔点较低而后在已经形成的NbB2表面形核,实现镍对NbB2颗粒的包覆。First, the pressure of the vacuum reaction chamber filled with inert gas is set at 0.01-0.03MPa, and a high-frequency power supply and a direct current power supply are used to generate a stable inert mixed gas thermal plasma. Subsequently, a mixture of micron nickel powder and micron NbB2 powder is sent into the reaction chamber at a speed of 3-20 m/s. When the high-energy density thermal plasma acts on the mixed powder, plasma is generated. During the diffusion process, the plasma continuously collides violently with the inert gas atoms, and then is rapidly cooled by a cooling device, spontaneously nucleates and condenses to grow into ultrafine particle clusters. After the clusters are formed, they quickly leave the supersaturated zone through gas convection, and finally deposit on the wall of the particle collection device. Due to the high melting point of NbB2 , it first nucleates and solidifies, and the nickel has a lower melting point and then nucleates on the surface of the already formed NbB2 , so that the nickel coating of the NbB2 particles is achieved.

(1c)镍包覆NbB2颗粒尺寸筛选和再细化加工:(1c) Nickel-coated NbB 2 particle size screening and further refinement processing:

筛选处理:收集步骤(1b)所制备的镍包覆NbB2颗粒粉体,将600纳米以下的颗粒筛选出来,作为成品;将颗粒尺寸大于600纳米作为原料,再经过步骤(1b)处理,直到收集的镍包覆NbB2颗粒粉体尺寸都为600纳米以下的为止。Screening treatment: Collect the nickel-coated NbB2 particle powder prepared in step (1b), and screen out particles below 600 nanometers as the finished product; use particles larger than 600 nanometers as raw materials and process them in step (1b) until the size of the collected nickel-coated NbB2 particle powder is all below 600 nanometers.

(2)真空感应熔炼镍包覆NbB2纳米颗粒增强NiAl合金:(2) Vacuum induction melting of nickel-coated NbB2 nanoparticles reinforced NiAl alloy:

(2a)将准备好的NiAl合金原料放入到水冷铜坩埚中,注意除坩埚底部,NiAl合金原料应避免与水冷铜坩埚壁接触,其次将步骤(1c)所得的镍包覆NbB2纳米颗粒和平衡NiAl配比所需补充的Al粉(含Al量为:99.8%)分别放入投料口中方便后续工作的开展;(2a) putting the prepared NiAl alloy raw material into a water-cooled copper crucible, and paying attention to avoiding contact between the NiAl alloy raw material and the water-cooled copper crucible wall except the bottom of the crucible, and then putting the nickel-coated NbB2 nanoparticles obtained in step (1c) and the Al powder (containing 99.8%) required to balance the NiAl ratio into the feeding port to facilitate the subsequent work;

(2b)开始熔炼前,使熔炼室内的真空度保持在5~20Pa,随后充入惰性气体,使熔炼室的压力保持在10000-20000Pa;(2b) Before starting smelting, the vacuum degree in the smelting chamber is maintained at 5-20 Pa, and then inert gas is filled to maintain the pressure of the smelting chamber at 10000-20000 Pa;

(2c)加热的功率不断地增加,每次提升3~7kW并保持5~8分钟,直至NiAl合金熔化;当NiAl合金全部熔化后,将投料口处的镍包覆NbB2纳米颗粒加入到水冷铜坩埚中NiAl合金熔体内;通过电磁感应不断地搅拌使得NbB2纳米颗粒在NiAl熔体中充分分散40~80秒后加入Al粉,3~7分钟后进行浇铸。(2c) The heating power is continuously increased by 3 to 7 kW each time and maintained for 5 to 8 minutes until the NiAl alloy is melted; when the NiAl alloy is completely melted, the nickel-coated NbB2 nanoparticles at the feeding port are added into the NiAl alloy melt in the water-cooled copper crucible; the NbB2 nanoparticles are continuously stirred by electromagnetic induction to fully disperse them in the NiAl melt, and then Al powder is added after 40 to 80 seconds, and casting is performed after 3 to 7 minutes.

(3)浇铸镍包覆NbB2纳米颗粒增强NiAl合金:(3) Cast nickel-coated NbB2 nanoparticles reinforced NiAl alloy:

(3a)利用石墨模具进行浇铸,熔炼时将其提前放在真空熔炼室中,距离水冷铜坩埚5厘米左右的位置,熔炼过程中同时对石墨模具进行充分预热处理,降低与浇铸NiAl合金之间的温差。(3a) A graphite mold is used for casting. During smelting, the mold is placed in a vacuum melting chamber in advance, about 5 cm away from a water-cooled copper crucible. During the smelting process, the graphite mold is fully preheated to reduce the temperature difference between the mold and the cast NiAl alloy.

(3b)当镍包覆包覆NbB2纳米颗粒分散均匀且补充好Al后,开始浇铸,浇铸时逐渐降低熔炼炉的功率至0;最后待NiAl合金冷却,即可使用。(3b) When the nickel-coated NbB2 nanoparticles are evenly dispersed and Al is supplemented, casting begins. During casting, the power of the smelting furnace is gradually reduced to 0; finally, the NiAl alloy is cooled and can be used.

其中,NbB2纳米颗粒的质量占增强的NiAl合金熔体总质量(最终制备的增强NiAl合金质量)的0.05~0.30wt.%。The mass of the NbB2 nanoparticles accounts for 0.05-0.30 wt.% of the total mass of the enhanced NiAl alloy melt (the mass of the enhanced NiAl alloy finally prepared).

实施例1Example 1

本实施例为真空感应熔炼法制备NbB2纳米颗粒增强的NiAl合金(由50at.%Ni和50at.%Al组成),NbB2纳米颗粒的质量占制备得到的增强NiAl合金总质量的0.05wt.%,具体方法如下:This embodiment is a NiAl alloy reinforced with NbB2 nanoparticles (composed of 50at.% Ni and 50at.% Al) prepared by vacuum induction melting, the mass of NbB2 nanoparticles accounts for 0.05wt.% of the total mass of the prepared reinforced NiAl alloy, and the specific method is as follows:

(1)高频感应等离子体制备镍包覆NbB2纳米颗粒;(1) Preparation of nickel-coated NbB2 nanoparticles by high-frequency induction plasma;

(1a)微米镍粉和微米NbB2粉体混合物配置和均匀混合:(1a) Preparation and uniform mixing of micron nickel powder and micron NbB2 powder mixture:

配置混合粉体,成分为:50wt%微米NbB2粉,NbB2粉体尺寸为20微米,纯度99.5wt%;50wt%微米镍粉,镍粉体尺寸为180微米,纯度99.5wt%;将配好的混合粉体放入球磨机内以60r/min的速度进行均匀化处理,混合60分钟;将球磨后的粉料取出,待用。Prepare a mixed powder, the ingredients of which are: 50wt% micron NbB2 powder, the NbB2 powder size is 20 microns, and the purity is 99.5wt%; 50wt% micron nickel powder, the nickel powder size is 180 microns, and the purity is 99.5wt%; put the prepared mixed powder into a ball mill for homogenization at a speed of 60r/min, and mix for 60 minutes; take out the ball-milled powder for standby use.

(1b)微米镍粉和微米NbB2粉体混合物经高频感应等离子体制备镍包覆NbB2纳米颗粒:(1b) Preparation of nickel-coated NbB2 nanoparticles by high-frequency induction plasma from a mixture of micron nickel powder and micron NbB2 powder:

首先使充入惰性气体的真空反应室的气压处于0.01MPa,利用高频电源和直流电源产生稳定的惰性混合气体热等离子体。随后以20米/秒的速度将微米镍粉和微米NbB2粉体混合物送进反应室,高能量密度热等离子体作用于混合粉体时,产生等离子体,该等离子体在扩散过程中,不断与惰性气体原子发生激烈的碰撞,然后利用冷却装置迅速冷却,自发成核并凝聚生长成超微粒团簇,团簇形成后,通过气体对流作用而迅速离开过饱和区,最后沉积在粒子收集装置的器壁,由于NbB2熔点高而先形核凝固,镍熔点较低而后在已经形成的NbB2表面形核,实现镍对NbB2颗粒的包覆。First, the pressure of the vacuum reaction chamber filled with inert gas is set at 0.01MPa, and a high-frequency power supply and a direct current power supply are used to generate a stable inert mixed gas thermal plasma. Subsequently, a mixture of micron nickel powder and micron NbB2 powder is sent into the reaction chamber at a speed of 20 m/s. When the high-energy density thermal plasma acts on the mixed powder, a plasma is generated. During the diffusion process, the plasma continuously collides violently with the inert gas atoms, and then is rapidly cooled by a cooling device, spontaneously nucleates and condenses to grow into ultrafine particle clusters. After the clusters are formed, they quickly leave the supersaturated zone through gas convection, and finally deposit on the wall of the particle collection device. Due to the high melting point of NbB2 , it first nucleates and solidifies, and the nickel has a lower melting point and then nucleates on the surface of the already formed NbB2 , thereby achieving nickel coating of the NbB2 particles.

(1c)镍包覆NbB2颗粒尺寸筛选和再细化加工:(1c) Nickel-coated NbB 2 particle size screening and further refinement processing:

筛选处理:收集步骤(1b)所制备的镍包覆NbB2颗粒粉体,将600纳米以下的颗粒筛选出来,作为成品;将颗粒尺寸大于600纳米作为原料,再经过步骤(1b)处理,直到收集的镍包覆NbB2颗粒粉体尺寸都为600纳米以下的为止。Screening treatment: Collect the nickel-coated NbB2 particle powder prepared in step (1b), and screen out particles below 600 nanometers as the finished product; use particles larger than 600 nanometers as raw materials and process them in step (1b) until the size of the collected nickel-coated NbB2 particle powder is all below 600 nanometers.

(2)真空感应熔炼镍包覆NbB2纳米颗粒增强NiAl合金:(2a)将准备好的NiAl合金原料放入到水冷铜坩埚中,注意除坩埚底部,NiAl合金原料应避免与水冷铜坩埚壁接触,其次将步骤(1c)所得的镍包覆NbB2纳米颗粒和平衡NiAl配比所需补充的Al粉(含Al量为:99.8%)分别放入投料口中方便后续工作的开展;(2) Vacuum induction melting of nickel-coated NbB2 nanoparticles to reinforce NiAl alloy: (2a) Place the prepared NiAl alloy raw material into a water-cooled copper crucible. Note that except for the bottom of the crucible, the NiAl alloy raw material should avoid contact with the wall of the water-cooled copper crucible. Then, place the nickel-coated NbB2 nanoparticles obtained in step (1c) and the Al powder (containing 99.8%) required to balance the NiAl ratio into the feeding port to facilitate subsequent work.

(2b)开始熔炼前,使熔炼室内的真空度保持在5Pa,随后充入惰性气体,使熔炼室的压力保持在15000Pa。(2b) Before starting smelting, the vacuum degree in the smelting chamber is maintained at 5 Pa, and then inert gas is filled to keep the pressure in the smelting chamber at 15000 Pa.

(2c)加热的功率不断地增加,每次提升3kW并保持6分钟直至NiAl合金熔化;当NiAl合金全部熔化后,将投料口处的镍包覆NbB2纳米颗粒加入到水冷铜坩埚中NiAl合金熔体内;通过电磁感应不断地搅拌使得NbB2纳米颗粒在NiAl熔体中充分分散40秒后加入Al粉,3分钟后进行浇铸。(2c) The heating power is continuously increased by 3 kW each time and maintained for 6 minutes until the NiAl alloy is melted; when the NiAl alloy is completely melted, the nickel-coated NbB2 nanoparticles at the feeding port are added into the NiAl alloy melt in the water-cooled copper crucible; the NbB2 nanoparticles are continuously stirred by electromagnetic induction to fully disperse them in the NiAl melt, and then Al powder is added after 40 seconds, and casting is carried out after 3 minutes.

(3)浇铸镍包覆NbB2纳米颗粒增强NiAl合金:(3) Cast nickel-coated NbB2 nanoparticles reinforced NiAl alloy:

(3a)利用石墨模具进行浇铸,熔炼时将其提前放在真空熔炼室中,距离水冷铜坩埚5厘米左右的位置,熔炼过程中同时对石墨模具进行充分预热处理,降低与浇铸NiAl合金之间的温差;(3a) Casting is performed using a graphite mold, which is placed in a vacuum melting chamber in advance at a distance of about 5 cm from a water-cooled copper crucible during smelting. During the smelting process, the graphite mold is fully preheated to reduce the temperature difference between the graphite mold and the cast NiAl alloy;

(3b)当镍包覆包覆NbB2纳米颗粒分散均匀且补充好Al后,开始浇铸,浇铸时逐渐降低熔炼炉的功率至0;最后待NiAl合金冷却,即可使用。(3b) When the nickel-coated NbB2 nanoparticles are evenly dispersed and Al is supplemented, casting begins. During casting, the power of the smelting furnace is gradually reduced to 0; finally, the NiAl alloy is cooled and can be used.

本实施例中,NiAl-0.05wt.%NbB2的显微组织如图2所示,可见NbB2陶瓷颗粒在镍铝基体中的分散情况良好,没有发生纳米颗粒的团聚,并且NbB2陶瓷颗粒与镍铝基体界面结合良好,没有空洞等缺陷。镍包覆NbB2纳米颗粒相组成如图3所示;镍包覆NbB2纳米颗粒的组织图如图4所示。当应变速率为1.0×10-4s时,600℃时的屈服强度、极限压缩强度和断裂应变分别为346.7MPa,438.2MPa,8.23%(表1),相较于未添加镍包覆NbB2纳米颗粒增强的NiAl合金分别增加8.2%,9.4%,10.3%。显然纳米颗粒不团聚,良好的分散及良好的界面结合,有利于纳米颗粒对镍铝合金力学性能的强化。In this embodiment, the microstructure of NiAl-0.05wt.% NbB2 is shown in Figure 2, and it can be seen that the dispersion of NbB2 ceramic particles in the nickel-aluminum matrix is good, there is no agglomeration of nanoparticles, and the interface of NbB2 ceramic particles and the nickel-aluminum matrix is well bonded, without defects such as cavities. The phase composition of nickel-coated NbB2 nanoparticles is shown in Figure 3; the organization diagram of nickel-coated NbB2 nanoparticles is shown in Figure 4. When the strain rate is 1.0× 10-4 s, the yield strength, ultimate compressive strength and fracture strain at 600°C are 346.7MPa, 438.2MPa, and 8.23% (Table 1), respectively, which are 8.2%, 9.4%, and 10.3% higher than the NiAl alloy reinforced by the nickel-coated NbB2 nanoparticles. Obviously, the nanoparticles do not agglomerate, have good dispersion and good interface bonding, which is conducive to the strengthening of the mechanical properties of the nickel-aluminum alloy by nanoparticles.

实施例2Example 2

本实施例为真空感应熔炼法制备NbB2纳米颗粒增强的NiAl合金(由50at.%Ni和50at.%Al组成),NbB2纳米颗粒的质量占制备得到的增强NiAl合金总质量的0.15wt.%,具体方法如下:This embodiment is a NiAl alloy reinforced with NbB2 nanoparticles (composed of 50at.% Ni and 50at.% Al) prepared by vacuum induction melting, the mass of NbB2 nanoparticles accounts for 0.15wt.% of the total mass of the prepared reinforced NiAl alloy, and the specific method is as follows:

(1)高频感应等离子体制备镍包覆NbB2纳米颗粒;(1) Preparation of nickel-coated NbB2 nanoparticles by high-frequency induction plasma;

(1a)微米镍粉和微米NbB2粉体混合物配置和均匀混合:(1a) Preparation and uniform mixing of micron nickel powder and micron NbB2 powder mixture:

配置混合粉体,成分为:80wt%微米NbB2粉,NbB2粉体尺寸为100微米,纯度99.5wt%;20wt%微米镍粉,镍粉体尺寸为200微米,纯度99.5wt%;将配好的混合粉体放入球磨机内以60r/min的速度进行均匀化处理,混合90分钟;将球磨后的粉料取出,待用。Prepare a mixed powder, the ingredients of which are: 80wt% micron NbB2 powder, the NbB2 powder size is 100 microns, and the purity is 99.5wt%; 20wt% micron nickel powder, the nickel powder size is 200 microns, and the purity is 99.5wt%; put the prepared mixed powder into a ball mill for homogenization at a speed of 60r/min, and mix for 90 minutes; take out the ball-milled powder for standby use.

(1b)微米镍粉和微米NbB2粉体混合物经高频感应等离子体制备镍包覆NbB2纳米颗粒:(1b) A mixture of micron nickel powder and micron NbB2 powder is subjected to high-frequency induction plasma to prepare nickel-coated NbB2 nanoparticles:

首先使充入惰性气体的真空反应室的气压处于0.02MPa,利用高频电源和直流电源产生稳定的惰性混合气体热等离子体。随后15米/秒的速度将微米镍粉和微米NbB2粉体混合物送进反应室,高能量密度热等离子体作用于混合粉体时,产生等离子体,该等离子体在扩散过程中,不断与惰性气体原子发生激烈的碰撞,然后利用冷却装置迅速冷却,自发成核并凝聚生长成超微粒团簇,团簇形成后,通过气体对流作用而迅速离开过饱和区,最后沉积在粒子收集装置的器壁,由于NbB2熔点高而先形核凝固,镍熔点较低而后在已经形成的NbB2表面形核,实现镍对NbB2颗粒的包覆。First, the pressure of the vacuum reaction chamber filled with inert gas is set at 0.02MPa, and a high-frequency power supply and a direct current power supply are used to generate a stable inert mixed gas thermal plasma. Then, a mixture of micron nickel powder and micron NbB2 powder is sent into the reaction chamber at a speed of 15 m/s. When the high-energy density thermal plasma acts on the mixed powder, a plasma is generated. During the diffusion process, the plasma continuously collides violently with the inert gas atoms, and then is rapidly cooled by a cooling device, spontaneously nucleates and condenses to grow into ultrafine particle clusters. After the clusters are formed, they quickly leave the supersaturated zone through gas convection, and finally deposit on the wall of the particle collection device. Due to the high melting point of NbB2 , it first nucleates and solidifies, and the nickel has a lower melting point and then nucleates on the surface of the already formed NbB2 , thereby achieving nickel coating of the NbB2 particles.

(1c)镍包覆NbB2颗粒尺寸筛选和再细化加工:(1c) Nickel-coated NbB 2 particle size screening and further refinement processing:

筛选处理:收集步骤(1b)所制备的镍包覆NbB2颗粒粉体,将600纳米以下的颗粒筛选出来,作为成品;将颗粒尺寸大于600纳米作为原料,再经过步骤(1b)处理,直到收集的镍包覆NbB2颗粒粉体尺寸都为600纳米以下的为止。Screening treatment: Collect the nickel-coated NbB2 particle powder prepared in step (1b), screen out particles below 600 nanometers as the finished product; use particles larger than 600 nanometers as raw materials, and then process them in step (1b) until the size of the collected nickel-coated NbB2 particle powder is all below 600 nanometers.

(2)真空感应熔炼镍包覆NbB2纳米颗粒增强NiAl合金:(2) Vacuum induction melting of nickel-coated NbB2 nanoparticles reinforced NiAl alloy:

(2a)将准备好的NiAl合金原料放入到水冷铜坩埚中,注意除坩埚底部,NiAl合金原料应避免与水冷铜坩埚壁接触,其次将步骤(1c)所得的镍包覆NbB2纳米颗粒和平衡NiAl配比所需补充的Al粉(含Al量为:99.8%)分别放入投料口中方便后续工作的开展;(2a) putting the prepared NiAl alloy raw material into a water-cooled copper crucible, and paying attention to avoiding contact between the NiAl alloy raw material and the water-cooled copper crucible wall except the bottom of the crucible, and then putting the nickel-coated NbB2 nanoparticles obtained in step (1c) and the Al powder (containing 99.8%) required to balance the NiAl ratio into the feeding port to facilitate the subsequent work;

(2b)开始熔炼前,使熔炼室内的真空度保持在20Pa,随后充入惰性气体,使熔炼室的压力保持在20000Pa。(2b) Before starting smelting, the vacuum degree in the smelting chamber is maintained at 20 Pa, and then inert gas is filled to keep the pressure in the smelting chamber at 20000 Pa.

(2c)加热的功率不断地增加,每次提升7kW并保持8分钟直至NiAl合金熔化;当NiAl合金全部熔化后,将投料口处的镍包覆NbB2纳米颗粒加入到水冷铜坩埚中NiAl合金熔体内;通过电磁感应不断地搅拌使得NbB2纳米颗粒在NiAl熔体中充分分散80秒后加入Al粉,7分钟后进行浇铸。(2c) The heating power is continuously increased by 7 kW each time and maintained for 8 minutes until the NiAl alloy is melted; when the NiAl alloy is completely melted, the nickel-coated NbB2 nanoparticles at the feeding port are added into the NiAl alloy melt in the water-cooled copper crucible; the NbB2 nanoparticles are continuously stirred by electromagnetic induction to fully disperse them in the NiAl melt, and then Al powder is added after 80 seconds, and casting is carried out after 7 minutes.

(3)浇铸镍包覆NbB2纳米颗粒增强NiAl合金:(3) Cast nickel-coated NbB2 nanoparticles reinforced NiAl alloy:

(3a)利用石墨模具进行浇铸,熔炼时将其提前放在真空熔炼室中,距离水冷铜坩埚5厘米左右的位置,熔炼过程中同时对石墨模具进行充分预热处理,降低与浇铸NiAl合金之间的温差;(3a) Casting is performed using a graphite mold, which is placed in a vacuum melting chamber in advance at a distance of about 5 cm from a water-cooled copper crucible during smelting. During the smelting process, the graphite mold is fully preheated to reduce the temperature difference between the graphite mold and the cast NiAl alloy;

(3b)当镍包覆包覆NbB2纳米颗粒分散均匀且补充好Al后,开始浇铸,浇铸时逐渐降低熔炼炉的功率至0;最后待NiAl合金冷却,即可使用。(3b) When the nickel-coated NbB2 nanoparticles are evenly dispersed and Al is supplemented, casting begins. During casting, the power of the smelting furnace is gradually reduced to 0; finally, the NiAl alloy is cooled and can be used.

本实施例中,NiAl-0.15wt.%NbB2的显微组织如图5所示,可见NbB2陶瓷颗粒在镍铝基体中的分散情况良好,没有发生纳米颗粒的团聚,并且NbB2陶瓷颗粒与镍铝基体界面结合良好,没有空洞等缺陷。0.15wt.%镍包覆NbB2纳米颗粒相组成如图6所示;镍包覆NbB2纳米颗的组织图如图7所示。当应变速率为1.0×10-4s时,600℃时的屈服强度、极限压缩强度和断裂应变分别为352.4MPa,446.5MPa,8.97%(表1),相较于未添加镍包覆NbB2纳米颗粒增强的NiAl合金分别增加10.0%,11.5%,20.2%。显然纳米颗粒不团聚,良好的分散及良好的界面结合,有利于纳米颗粒对镍铝合金力学性能的强化。In this embodiment, the microstructure of NiAl-0.15wt.% NbB 2 is shown in FIG5 , and it can be seen that the dispersion of NbB 2 ceramic particles in the nickel-aluminum matrix is good, and there is no agglomeration of nanoparticles, and the NbB 2 ceramic particles are well bonded to the interface of the nickel-aluminum matrix, and there are no defects such as voids. The phase composition of 0.15wt.% nickel-coated NbB 2 nanoparticles is shown in FIG6 ; the organization diagram of nickel-coated NbB 2 nanoparticles is shown in FIG7 . When the strain rate is 1.0×10 -4 s, the yield strength, ultimate compressive strength and fracture strain at 600°C are 352.4MPa, 446.5MPa, and 8.97% (Table 1), respectively, which are 10.0%, 11.5%, and 20.2% higher than the NiAl alloy reinforced by the nickel-coated NbB 2 nanoparticles without addition. Obviously, the nanoparticles do not agglomerate, and the good dispersion and good interface bonding are conducive to the strengthening of the mechanical properties of the nickel-aluminum alloy by the nanoparticles.

实施例3Example 3

本实施例为真空感应熔炼法制备NbB2纳米颗粒增强的NiAl合金(由50at.%Ni和50at.%Al组成),NbB2纳米颗粒的质量占制备得到的增强NiAl合金总质量的0.30wt.%,具体方法如下:This embodiment is a NiAl alloy reinforced with NbB2 nanoparticles (composed of 50at.% Ni and 50at.% Al) prepared by vacuum induction melting, the mass of NbB2 nanoparticles accounts for 0.30wt.% of the total mass of the prepared reinforced NiAl alloy, and the specific method is as follows:

(1)高频感应等离子体制备镍包覆NbB2纳米颗粒;(1) Preparation of nickel-coated NbB2 nanoparticles by high-frequency induction plasma;

(1a)微米镍粉和微米NbB2粉体混合物配置和均匀混合:(1a) Preparation and uniform mixing of micron nickel powder and micron NbB2 powder mixture:

配置混合粉体,成分为:70wt%微米NbB2粉,NbB2粉体尺寸为10微米,纯度99.5wt%;30wt%微米镍粉,镍粉体尺寸为20微米,纯度99.5wt%;将配好的混合粉体放入球磨机内以30r/min的速度进行均匀化处理,混合50分钟;将球磨后的粉料取出,待用。Prepare a mixed powder, the ingredients of which are: 70wt% micron NbB2 powder, the NbB2 powder size is 10 microns, and the purity is 99.5wt%; 30wt% micron nickel powder, the nickel powder size is 20 microns, and the purity is 99.5wt%; put the prepared mixed powder into a ball mill for homogenization at a speed of 30r/min, and mix for 50 minutes; take out the ball-milled powder for standby use.

(1b)微米镍粉和微米NbB2粉体混合物经高频感应等离子体制备镍包覆NbB2纳米颗粒:(1b) Preparation of nickel-coated NbB2 nanoparticles by high-frequency induction plasma from a mixture of micron nickel powder and micron NbB2 powder:

首先使充入惰性气体的真空反应室的气压处于0.03MPa,利用高频电源和直流电源产生稳定的惰性混合气体热等离子体。随10米/秒的速度将微米镍粉和微米NbB2粉体混合物送进反应室,高能量密度热等离子体作用于混合粉体时,产生等离子体,该等离子体在扩散过程中,不断与惰性气体原子发生激烈的碰撞,然后利用冷却装置迅速冷却,自发成核并凝聚生长成超微粒团簇,团簇形成后,通过气体对流作用而迅速离开过饱和区,最后沉积在粒子收集装置的器壁,由于NbB2熔点高而先形核凝固,镍熔点较低而后在已经形成的NbB2表面形核,实现镍对NbB2颗粒的包覆。First, the pressure of the vacuum reaction chamber filled with inert gas is set at 0.03MPa, and a high-frequency power supply and a direct current power supply are used to generate a stable inert mixed gas thermal plasma. A mixture of micron nickel powder and micron NbB2 powder is sent into the reaction chamber at a speed of 10 m/s. When the high-energy density thermal plasma acts on the mixed powder, plasma is generated. During the diffusion process, the plasma continuously collides violently with the inert gas atoms, and then is rapidly cooled by a cooling device, spontaneously nucleates and condenses to grow into ultrafine particle clusters. After the clusters are formed, they quickly leave the supersaturated zone through gas convection, and finally deposit on the wall of the particle collection device. Due to the high melting point of NbB2 , it first nucleates and solidifies, and nickel has a lower melting point and then nucleates on the surface of the already formed NbB2 , thereby achieving nickel coating of NbB2 particles.

(1c)镍包覆NbB2颗粒尺寸筛选和再细化加工:(1c) Nickel-coated NbB 2 particle size screening and further refinement processing:

筛选处理:收集步骤(1b)所制备的镍包覆NbB2颗粒粉体,将600纳米以下的颗粒筛选出来,作为成品;将颗粒尺寸大于600纳米作为原料,再经过步骤(1b)处理,直到收集的镍包覆NbB2颗粒粉体尺寸都为600纳米以下的为止。Screening treatment: Collect the nickel-coated NbB2 particle powder prepared in step (1b), and screen out particles below 600 nanometers as the finished product; use particles larger than 600 nanometers as raw materials and process them in step (1b) until the size of the collected nickel-coated NbB2 particle powder is all below 600 nanometers.

(2)真空感应熔炼镍包覆NbB2纳米颗粒增强NiAl合金:(2) Vacuum induction melting of nickel-coated NbB2 nanoparticles reinforced NiAl alloy:

(2a)将准备好的NiAl合金原料放入到水冷铜坩埚中,注意除坩埚底部,NiAl合金原料应避免与水冷铜坩埚壁接触,其次将步骤(1c)所得的镍包覆NbB2纳米颗粒和平衡NiAl配比所需补充的Al粉(含Al量为:99.8%)分别放入投料口中方便后续工作的开展;(2a) putting the prepared NiAl alloy raw material into a water-cooled copper crucible, and paying attention to avoiding contact between the NiAl alloy raw material and the water-cooled copper crucible wall except the bottom of the crucible, and then putting the nickel-coated NbB2 nanoparticles obtained in step (1c) and the Al powder (containing 99.8%) required to balance the NiAl ratio into the feeding port to facilitate the subsequent work;

(2b)开始熔炼前,使熔炼室内的真空度保持15Pa,随后充入惰性气体,使熔炼室的压力保持在12000Pa。(2b) Before starting smelting, the vacuum degree in the smelting chamber is maintained at 15 Pa, and then inert gas is filled to keep the pressure in the smelting chamber at 12000 Pa.

(2c)加热的功率不断地增加,每次提升4kW并保持7分钟直至NiAl合金熔化;当NiAl合金全部熔化后,将投料口处的镍包覆NbB2纳米颗粒加入到水冷铜坩埚中NiAl合金熔体内;通过电磁感应不断地搅拌使得NbB2纳米颗粒在NiAl熔体中充分分散60秒后加入Al粉,5分钟后进行浇铸。(2c) The heating power is continuously increased by 4 kW each time and maintained for 7 minutes until the NiAl alloy is melted; when the NiAl alloy is completely melted, the nickel-coated NbB2 nanoparticles at the feeding port are added into the NiAl alloy melt in the water-cooled copper crucible; the NbB2 nanoparticles are continuously stirred by electromagnetic induction to fully disperse them in the NiAl melt, and then Al powder is added after 60 seconds, and casting is carried out after 5 minutes.

(3)浇铸镍包覆NbB2纳米颗粒增强NiAl合金:(3) Cast nickel-coated NbB2 nanoparticles reinforced NiAl alloy:

(3a)利用石墨模具进行浇铸,熔炼时将其提前放在真空熔炼室中,距离水冷铜坩埚5厘米左右的位置,熔炼过程中同时对石墨模具进行充分预热处理,降低与浇铸NiAl合金之间的温差;(3a) Casting is performed using a graphite mold, which is placed in a vacuum melting chamber in advance at a distance of about 5 cm from a water-cooled copper crucible during smelting. During the smelting process, the graphite mold is fully preheated to reduce the temperature difference between the graphite mold and the cast NiAl alloy;

(3b)当镍包覆包覆NbB2纳米颗粒分散均匀且补充好Al后,开始浇铸,浇铸时逐渐降低熔炼炉的功率至0;最后待NiAl合金冷却,即可使用。(3b) When the nickel-coated NbB2 nanoparticles are evenly dispersed and Al is supplemented, casting begins. During casting, the power of the smelting furnace is gradually reduced to 0; finally, the NiAl alloy is cooled and can be used.

本实施例中,NiAl-0.3wt.%NbB2的显微组织如图8所示,可见NbB2陶瓷颗粒在镍铝基体中的分散情况良好,没有发生纳米颗粒的团聚,并且NbB2陶瓷颗粒与镍铝基体界面结合良好,没有空洞等缺陷。0.3wt.%镍包覆NbB2纳米颗粒相组成如图9所示;镍包覆NbB2纳米颗的组织图如图10所示。当应变速率为1.0×10-4s时,600℃时的屈服强度、极限压缩强度和断裂应变分别为349.3MPa,441.5MPa,8.31%(表1),相较于未添加镍包覆NbB2纳米颗粒增强的NiAl合金分别增加9.0%,10.2%,11.4%。显然纳米颗粒不团聚,良好的分散及良好的界面结合,有利于纳米颗粒对镍铝合金力学性能的强化。In this embodiment, the microstructure of NiAl-0.3wt.% NbB2 is shown in Figure 8, which shows that the dispersion of NbB2 ceramic particles in the nickel-aluminum matrix is good, there is no agglomeration of nanoparticles, and the interface of NbB2 ceramic particles and the nickel-aluminum matrix is well bonded, without defects such as voids. The phase composition of 0.3wt.% nickel-coated NbB2 nanoparticles is shown in Figure 9; the organization diagram of nickel-coated NbB2 nanoparticles is shown in Figure 10. When the strain rate is 1.0× 10-4 s, the yield strength, ultimate compressive strength and fracture strain at 600℃ are 349.3MPa, 441.5MPa, and 8.31% (Table 1), respectively, which are 9.0%, 10.2%, and 11.4% higher than those of NiAl alloys reinforced with no nickel-coated NbB2 nanoparticles. Obviously, the nanoparticles do not agglomerate, have good dispersion and good interface bonding, which is conducive to the strengthening of the mechanical properties of nickel-aluminum alloys by nanoparticles.

对比例1Comparative Example 1

真空感应熔炼法制备空白的NiAl合金(由50at.%Ni和50at.%Al组成),具体方法如下。A blank NiAl alloy (composed of 50 at. % Ni and 50 at. % Al) was prepared by vacuum induction melting, and the specific method is as follows.

(1)真空感应熔炼NiAl合金:(1) Vacuum induction melting of NiAl alloy:

(1a)将NiAl合金原料放入到水冷铜坩埚中,注意除坩埚底部,NiAl合金原料应避免与水冷铜坩埚壁接触;(1a) Put the NiAl alloy raw material into a water-cooled copper crucible, and pay attention to avoid contact between the NiAl alloy raw material and the water-cooled copper crucible wall except the bottom of the crucible;

(1b)为了避免材料氧化,使熔炼室内的真空度保持在10Pa,随后充入惰性气体,使熔炼室的压力保持在10000Pa;(1b) To prevent oxidation of the material, the vacuum degree in the smelting chamber is maintained at 10 Pa, and then an inert gas is filled to maintain the pressure in the smelting chamber at 10000 Pa;

(1c)加热的功率不断地增加,每次提升5kW并保持5分钟直至NiAl合金熔化。(1c) The heating power is continuously increased by 5 kW each time and maintained for 5 minutes until the NiAl alloy melts.

(2)浇铸NiAl合金:(2) Casting NiAl alloy:

(2a)利用石墨模具进行浇铸,熔炼时将其提前放在真空熔炼室中,距离水冷铜坩埚5厘米左右的位置,熔炼过程中同时对石墨模具进行充分预热处理,降低与浇铸NiAl合金之间的温差;(2a) Casting is performed using a graphite mold, which is placed in a vacuum melting chamber in advance during smelting, about 5 cm away from a water-cooled copper crucible. During the smelting process, the graphite mold is fully preheated to reduce the temperature difference between the graphite mold and the cast NiAl alloy;

(2b)开始浇铸,浇铸时逐渐降低熔炼炉的功率至0;最后待NiAl合金冷却,即可使用。(2b) Start casting and gradually reduce the power of the melting furnace to 0 during casting; finally, wait for the NiAl alloy to cool down before use.

本对比例中,NiAl的显微组织(如图1所示)。当应变速率为1.0×10-4s时,600℃时的屈服强度、极限压缩强度和断裂应变分别为320.4MPa,400.5MPa,7.46%(表1)。In this comparative example, the microstructure of NiAl (as shown in FIG. 1 ) is as follows: When the strain rate is 1.0×10 -4 s, the yield strength, ultimate compressive strength and fracture strain at 600° C. are 320.4 MPa, 400.5 MPa and 7.46% respectively (Table 1).

表1各实施例和对比例中制备的合金的压缩性能表Table 1 Compression performance of alloys prepared in various embodiments and comparative examples

本发明通过真空感应熔炼法制备镍包覆NbB2纳米颗粒增强NiAl合金,能够显著提高NiAl合金的性能。本发明提供的制备方法可大批量制备镍包覆纳米颗粒,表面包覆金属有利于纳米颗粒和NiAl熔体的润湿,有利于陶瓷颗粒在金属熔体中的分散,提高了陶瓷颗粒与NiAl基体间的界面结合。本发明制备过程简单易控制和自动化;能够纳米颗粒在金属熔体中分散的问题。The invention prepares nickel-coated NbB2 nanoparticle-reinforced NiAl alloy by vacuum induction melting, and can significantly improve the performance of NiAl alloy. The preparation method provided by the invention can prepare nickel-coated nanoparticles in large quantities, and the surface coating of metal is conducive to the wetting of nanoparticles and NiAl melt, and is conducive to the dispersion of ceramic particles in the metal melt, and improves the interface bonding between ceramic particles and NiAl matrix. The preparation process of the invention is simple, easy to control and automatic; and the problem of dispersion of nanoparticles in the metal melt can be solved.

尽管本发明的实施方案已公开如上,但其并不仅仅限于说明书和实施方式中所列运用,它完全可以被适用于各种适合本发明的领域,对于熟悉本领域的人员而言,可容易地实现另外的修改,因此在不背离权利要求及等同范围所限定的一般概念下,本发明并不限于特定的细节和这里示出与描述的图例。Although the embodiments of the present invention have been disclosed as above, they are not limited to the applications listed in the specification and the implementation modes, and they can be fully applied to various fields suitable for the present invention. For those familiar with the art, additional modifications can be easily implemented. Therefore, without departing from the general concept defined by the claims and the scope of equivalents, the present invention is not limited to the specific details and the illustrations shown and described herein.

Claims (9)

1. The preparation method of the nano NbB 2 particle reinforced NiAl alloy is characterized by comprising the following steps of:
step one, preparing nickel-coated NbB 2 nano particles;
Secondly, placing a NiAl alloy raw material into a water-cooled copper crucible in a smelting chamber of vacuum smelting equipment, and respectively placing the nickel-coated NbB 2 nano particles and Al powder into a feed port of the smelting chamber of the vacuum smelting equipment;
wherein the vacuum degree in the smelting chamber is kept between 5Pa and 20Pa;
step three, filling inert gas into the smelting chamber to keep the pressure of the smelting chamber at 10000 Pa-20000 Pa; heating the smelting chamber, and gradually increasing the heating power until the NiAl alloy is completely melted to obtain a NiAl alloy melt;
Step four, nickel coated NbB 2 nano particles at a feed port are added into a NiAl alloy melt in a water-cooled copper crucible; after fully dispersing NbB 2 nano particles in the NiAl melt by electromagnetic induction stirring, adding Al powder to obtain an enhanced NiAl alloy melt;
Wherein the mass of the NbB 2 nano-particles accounts for 0.05 to 0.30wt.% of the total mass of the reinforced NiAl alloy melt;
Step five, in the smelting chamber, casting the reinforced NiAl alloy melt by using a grinding tool; after casting and cooling, obtaining the nano NbB 2 particle reinforced NiAl alloy;
In the first step, nickel-coated NbB 2 nano-particles are prepared, and the method comprises the following steps:
Step 1, mixing nickel powder and NbB 2 powder, and homogenizing in a ball mill to obtain mixed powder;
Wherein, the grain diameter of the nickel powder is 20-200 microns, and the grain diameter of the NbB 2 powder is 10-100 microns; in the mixed powder, the nickel powder accounts for 20-50 wt%;
Step 2, filling inert gas into the vacuum reaction chamber, and generating stable inert gas mixed thermal plasma by using a high-frequency direct-current power supply; the mixed powder is sent into the vacuum reaction chamber, reacts after the thermal plasma, and is rapidly cooled to obtain nickel-coated NbB 2 powder;
And 3, screening particles below 600 nanometers from the nickel-coated NbB 2 powder, namely the nickel-coated NbB 2 nanometer particles.
2. The method for producing nano NbB 2 particle reinforced NiAl alloy according to claim 1, wherein in the step 2, the gas pressure of the vacuum reaction chamber filled with inert gas is 0.01MPa to 0.03MPa.
3. The method of preparing nano NbB 2 particle reinforced NiAl alloy according to claim 2, wherein in step 2, the mixed powder is fed into the vacuum reaction chamber at a speed of 3 m/s to 20 m/s.
4. A method of preparing a nano NbB 2 particle reinforced NiAl alloy according to any one of claims 1 to 3, wherein during the preparation of the NiAl alloy melt in step three, the heating power is raised by 3kW to 7kW each time and maintained for 5 to 8 minutes.
5. The method for producing nano NbB 2 particle reinforced NiAl alloy according to claim 4, wherein in the fourth step, after the nano NbB 2 particles are fully dispersed in the NiAl melt for 40 to 80 seconds, al powder is added.
6. The method for producing nano NbB 2 particle reinforced NiAl alloy according to claim 5, wherein in the fourth step, casting is performed after adding Al powder for 3 to 7 minutes.
7. The method for producing nano-NbB 2 particle reinforced NiAl alloy according to claim 6, wherein in the fifth step, the power of the melting equipment is gradually reduced to 0 during the casting process.
8. The method of preparing a nano NbB 2 particle reinforced NiAl alloy as claimed in claim 7, wherein in the fifth step, casting is performed using a graphite mold.
9. The method of producing nano NbB 2 particle reinforced NiAl alloy according to claim 8, wherein in step five, the method further comprises preheating the mold in a vacuum melting chamber before casting.
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