CN101259536A - A method for preparing high niobium titanium aluminum alloy powder - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 47
- 239000000843 powder Substances 0.000 title claims abstract description 47
- 229910000838 Al alloy Inorganic materials 0.000 title abstract description 12
- -1 niobium titanium aluminum Chemical compound 0.000 title description 6
- 238000009689 gas atomisation Methods 0.000 claims abstract description 20
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011261 inert gas Substances 0.000 claims abstract description 17
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 15
- 239000010955 niobium Substances 0.000 claims abstract description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 12
- 239000000956 alloy Substances 0.000 claims abstract description 12
- 230000006698 induction Effects 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000002844 melting Methods 0.000 claims abstract description 7
- 230000008018 melting Effects 0.000 claims abstract description 7
- 229910052786 argon Inorganic materials 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000007514 turning Methods 0.000 claims abstract description 6
- 238000003754 machining Methods 0.000 claims abstract description 5
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 238000004321 preservation Methods 0.000 claims abstract description 3
- 238000003723 Smelting Methods 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 7
- 238000004663 powder metallurgy Methods 0.000 abstract description 6
- 238000000265 homogenisation Methods 0.000 abstract description 3
- 238000003672 processing method Methods 0.000 abstract 1
- 229910010038 TiAl Inorganic materials 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000000889 atomisation Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 229910000765 intermetallic Inorganic materials 0.000 description 3
- 238000009690 centrifugal atomisation Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910006281 γ-TiAl Inorganic materials 0.000 description 1
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Abstract
本发明属于粉末冶金技术领域，特别是提供了一种高铌钛铝合金粉末的制备方法。原料采用铸态高铌钛铝基合金铸锭，工艺流程为：熔炼→均热化处理→车削加工→机加工成可以连接的棒材→无坩埚感应加热连续惰性气体雾化法，具体步骤为：(1)熔炼采用等离子冷床工艺；(2)在1100－1300℃保温24－48小时，进行均热化处理；然后将铸锭的表面氧化皮去除；(3)采用的线切割和机加工方法将铸锭加工成以螺纹连接的直径为20－25mm长度为200－500mm的棒材，然后进行车削处理去除棒材表面的氧化铁皮；(4)采用无坩埚感应加热连续惰性气体雾化工艺将棒材制成粉末，工艺参数为惰性气体压力2.0－5.0MPa，氩气流量160－220Ls－1。本发明的优点在于所制备的粉末球形度很好，纯度高，具有很好的流动性而且粉末收得率高。所制备的粉末球形度达到80－95％，粉末收得率75－85％。
The invention belongs to the technical field of powder metallurgy, and in particular provides a preparation method of high-niobium titanium-aluminum alloy powder. The raw material is cast high-niobium titanium-aluminum-based alloy ingot, and the process flow is: melting → soaking treatment → turning processing → machining into rods that can be connected → no crucible induction heating continuous inert gas atomization method, the specific steps are as follows: (1) Plasma cooling bed process is used for smelting; (2) heat preservation is carried out at 1100-1300°C for 24-48 hours, and homogenization treatment is carried out; then the surface scale of the ingot is removed; (3) wire cutting and machine The processing method is to process the ingot into a rod with a diameter of 20-25mm and a length of 200-500mm connected by threads, and then perform turning treatment to remove the iron oxide scale on the surface of the rod; (4) adopt continuous inert gas atomization without crucible induction heating Process The bar is made into powder, the process parameters are inert gas pressure 2.0-5.0MPa, argon flow rate 160-220Ls -1 . The invention has the advantages that the prepared powder has good sphericity, high purity, good fluidity and high powder yield. The sphericity of the prepared powder reaches 80-95%, and the powder yield is 75-85%.
Description
技术领域 technical field
本发明属于粉末冶金技术领域，特别是提供了一种高铌钛铝合金粉末的制备方法。具体是以高铌钛铝合金铸锭为原料采用无坩埚感应加热连续惰性气体雾化工艺制成粉末的制备方法。The invention belongs to the technical field of powder metallurgy, and in particular provides a preparation method of high-niobium titanium-aluminum alloy powder. Specifically, a high-niobium-titanium-aluminum alloy ingot is used as a raw material to prepare a powder by adopting a crucible-less induction heating continuous inert gas atomization process.
背景技术 Background technique
为提高航空和航天飞行器的工作效率，必须增加推力和节省燃料，提高发动机的工作温度和减轻飞行器的重量。因此，航空和航天发动机的选材应具备“更轻、更刚、更强和更耐热”的特性。具有低密度、高熔点、高弹性模量，有一定塑性的金属间化合物材料在最近二十多年得到广泛关注，成为提供这些特性的最佳材料之一。In order to improve the working efficiency of aviation and aerospace vehicles, it is necessary to increase the thrust and save fuel, increase the working temperature of the engine and reduce the weight of the aircraft. Therefore, the material selection of aviation and aerospace engines should have the characteristics of "lighter, stiffer, stronger and more heat-resistant". Intermetallic compound materials with low density, high melting point, high elastic modulus, and certain plasticity have attracted extensive attention in the past two decades, and have become one of the best materials to provide these properties.
γ-TiAl基金属间化合物由于其密度低，具有高的比强度和比弹性模量，在高温时仍可以保持足够高的强度和刚度，同时它还具有良好的抗蠕变及氧化能力，具有在下个十年推动结构材料变革的潜力，被认为是一种极具应用潜力的高温结构材料。高Nb-TiAl合金以其优良的抗氧化性能，高的室温和高温强度及耐高温蠕变性能成为新一代TiAl合金。Because of its low density, γ-TiAl-based intermetallic compound has high specific strength and specific elastic modulus, it can still maintain high enough strength and rigidity at high temperature, and it also has good creep and oxidation resistance. The potential to promote structural material change in the next decade is considered to be a high-temperature structural material with great application potential. High Nb-TiAl alloys have become a new generation of TiAl alloys due to their excellent oxidation resistance, high room temperature and high temperature strength and high temperature creep resistance.
由于TiAl合金室温塑性低，韧度差，难于机加工，至今仍是大量生产TiAl零件的主要障碍。目前高铌钛铝合金的制备以铸锭冶金为主，在采用等离子冷床熔炼和自耗凝壳的铸锭中，所得铸锭组织粗大，有黑色L偏析。Due to the low room temperature plasticity and poor toughness of TiAl alloy, it is difficult to machine, which is still the main obstacle to the mass production of TiAl parts. At present, the preparation of high-niobium titanium-aluminum alloy is mainly based on ingot metallurgy. In the ingots smelted by plasma cooling bed and consumable solidification shell, the obtained ingots have a coarse structure and black L segregation.
采用粉末冶金方法可制取近终形的TiAl基合金制品，能有效解决TiAl金属间化合物加工成形的困难，但是粉末的制备是粉末冶金方法的前提和基础。由于高铌钛铝室温塑性低，加工成形困难，所以采用粉末冶金方法可以制备近终成形零件解决高铌钛铝成形问题。The powder metallurgy method can be used to produce near-net-shaped TiAl-based alloy products, which can effectively solve the difficulty of processing and forming TiAl intermetallic compounds, but the powder preparation is the premise and basis of the powder metallurgy method. Due to the low plasticity of high niobium titanium aluminum at room temperature and the difficulty of processing and forming, the powder metallurgy method can be used to prepare near-net-shaped parts to solve the forming problem of high niobium titanium aluminum.
常规钛铝粉末制备主要采用机械粉碎法和雾化法。由于机械粉碎法制得的钛铝合金粉末氧含量偏高，其使用率呈下降趋势。雾化法又分为惰性气体雾化法和立新雾化法。离心雾化法中用于制备钛铝合金粉末的以旋转电极雾化法偏多。但是离心雾化法虽然制备的粉末纯度较高，但是粉末太粗，细粉率太低，在后续加工中不好使用。所以常规钛铝粉末制备以惰性气体雾化为主。气体雾化法是利用高压气体作为雾化介质来破碎连续的熔融金属细流。气体雾化法可以获得直径50～100μm的金属粉末，气体雾化粉为光滑圆球形，冷却速率为102～103℃/s。气体雾化法又分有坩锅气体雾化法和无坩锅气体雾化法。Conventional titanium aluminum powder is mainly prepared by mechanical pulverization and atomization. Due to the high oxygen content of the titanium-aluminum alloy powder prepared by the mechanical pulverization method, its utilization rate shows a downward trend. The atomization method is divided into inert gas atomization method and Lixin atomization method. In the centrifugal atomization method, the rotating electrode atomization method is mostly used to prepare titanium-aluminum alloy powder. However, although the powder prepared by the centrifugal atomization method has high purity, the powder is too coarse and the fine powder rate is too low, so it is not easy to use in subsequent processing. Therefore, the conventional preparation of titanium aluminum powder is mainly based on inert gas atomization. The gas atomization method uses high-pressure gas as the atomization medium to break up a continuous stream of molten metal. The gas atomization method can obtain metal powder with a diameter of 50-100 μm, the gas atomization powder is smooth and spherical, and the cooling rate is 10 2 -10 3 ℃/s. The gas atomization method is divided into crucible gas atomization method and crucible gas atomization method.
有坩埚气体雾化法是在坩埚中将金属熔化后，金属熔液流过细的喷嘴滴下时吹入高速旋转气体制取粉末的方法。TiAl合金是高熔点活性金属，而且对组织非常敏感，在坩埚中熔化时易污染，无法保持纯度。The crucible gas atomization method is to melt the metal in the crucible, and blow the high-speed rotating gas into the powder when the molten metal flows through a thin nozzle and drops. TiAl alloy is an active metal with a high melting point, and is very sensitive to the structure. It is easy to contaminate when it is melted in the crucible, and the purity cannot be maintained.
发明内容 Contents of the invention
本发明的目的在于以高铌钛铝铸锭为原料制备纯净的高铌钛铝粉末，为采用粉末冶金工艺制备复杂形状的钛铝合金零件提供原料保证。The purpose of the present invention is to prepare pure high-niobium titanium-aluminum powder by using high-niobium titanium-aluminum ingot as raw material, so as to provide raw material guarantee for preparing complex-shaped titanium-aluminum alloy parts by powder metallurgy technology.
由于高铌钛铝熔点较高，而且为了得到低杂质含量的粉末，采用无坩埚感应加热连续惰性气体雾化工艺。Due to the high melting point of high niobium titanium aluminum, and in order to obtain powder with low impurity content, a continuous inert gas atomization process without crucible induction heating is adopted.
一种高铌钛铝合金粉末的制备方法，原料采用铸态高铌钛铝基合金铸锭，化学成分原子百分比at.％为：Al：45-46％，Nb：5-10％，W：0.2-1％，Y：0.01-0.1％，余量为Ti；A method for preparing high-niobium titanium-aluminum alloy powder. The raw material is cast high-niobium titanium-aluminum alloy ingot, and the chemical composition atomic percentage at.% is: Al: 45-46%, Nb: 5-10%, W: 0.2-1%, Y: 0.01-0.1%, the balance is Ti;
本发明的工艺流程如下：Process flow of the present invention is as follows:
熔炼→均热化处理→车削加工→机加工成可以连接的棒材→无坩埚感应加热连续惰性气体雾化制粉Melting→homothermal treatment→turning→machining into rods that can be connected→induction heating without crucible and continuous inert gas atomization powder making
具体工艺步骤为：The specific process steps are:
熔炼：采用等离子冷床工艺制备铸锭Melting: Prepare ingots by plasma cooling bed process
均匀化处理：在1100-1300℃保温24-48小时，进行均热化处理；Homogenization treatment: heat preservation at 1100-1300°C for 24-48 hours, and perform homogenization treatment;
车削加工：将退火后的铸锭的表面氧化皮去除；Turning: remove the oxide skin on the surface of the annealed ingot;
棒材制备：采用的线切割和机加工方法将铸锭加工成以螺纹连接的直径为20-25mm长度为200-500mm的棒材，然后进行车削处理去除棒材表面的氧化铁皮；Bar preparation: The wire cutting and machining methods are used to process the ingot into a bar with a diameter of 20-25mm and a length of 200-500mm connected by threads, and then turn it to remove the iron oxide scale on the surface of the bar;
粉末制备：采用无坩埚感应加热连续惰性气体雾化工艺将高铌钛铝合金棒材制成粉末。工艺参数为惰性气体压力2.0-5.0MPa，氩气流量160-220Ls-1。Powder preparation: The high-niobium titanium-aluminum alloy rod is made into powder by using a crucible-free induction heating continuous inert gas atomization process. The process parameters are inert gas pressure 2.0-5.0MPa, argon flow rate 160-220Ls -1 .
无坩埚气体雾化法是将细长的TiAl合金棒通过感应圈缓慢下降，感应加热熔化的液体被来自喷嘴的氩或氦气雾化成粉。改变熔化金属的体积、雾化气的压力、流量和喷嘴的形状等参数可以控制粉末的粒度。由于熔化的金属不与坩埚和其它器皿接触，粉末不被污染，可制取低氧高纯TiAl合金粉。The non-crucible gas atomization method is to slowly drop the slender TiAl alloy rod through the induction coil, and the molten liquid heated by induction is atomized into powder by the argon or helium gas from the nozzle. The particle size of the powder can be controlled by changing parameters such as the volume of the molten metal, the pressure of the atomizing gas, the flow rate and the shape of the nozzle. Because the molten metal is not in contact with the crucible and other vessels, the powder is not polluted, and low-oxygen high-purity TiAl alloy powder can be produced.
本发明的优点在于所制备的粉末球形度很好，纯度高，具有很好的流动性而且粉末收得率高。所制备的粉末球形度达到80-95％，粉末收得率75-85％。当粒度为-200目时，合金粉中的氧含量为1150ppm。The invention has the advantages that the prepared powder has good sphericity, high purity, good fluidity and high powder yield. The sphericity of the prepared powder reaches 80-95%, and the powder yield is 75-85%. When the particle size is -200 mesh, the oxygen content in the alloy powder is 1150ppm.
附图说明 Description of drawings
图1为高铌钛铝粉末形貌。Figure 1 shows the morphology of high niobium titanium aluminum powder.
图2为高铌钛铝粉末粒度分布曲线。Figure 2 is the particle size distribution curve of high niobium titanium aluminum powder.
具体实施方式 Detailed ways
实施例1Example 1
采用等离子冷床工艺熔炼高铌钛铝铸锭，在1200℃保温24小时，进行均热化处理；然后将铸锭的表面氧化皮去除；采用的线切割方法将铸锭加工成可以连接的直径为20mm长度为220mm的棒材，然后进行车削处理去除棒材表面的氧化铁皮；采用无坩埚感应加热连续惰性气体雾化工艺将棒材制成粉末，工艺参数为惰性气体压力3.0MPa，氩气流量180Ls-1。所制备的粉末球形度达到92％，粉末收得率85％。当粒度为-200目时，合金粉中的氧含量为1150ppm。Use plasma cooling bed process to melt high-niobium titanium-aluminum ingot, keep it at 1200°C for 24 hours, and carry out soaking treatment; then remove the surface oxide scale of the ingot; use the wire cutting method to process the ingot into a diameter that can be connected It is a bar with a length of 20mm and a length of 220mm, and then it is turned to remove the iron oxide scale on the surface of the bar; the bar is made into powder by a continuous inert gas atomization process without crucible induction heating, and the process parameters are inert gas pressure 3.0MPa, argon Flow 180Ls -1 . The sphericity of the prepared powder reaches 92%, and the powder yield is 85%. When the particle size is -200 mesh, the oxygen content in the alloy powder is 1150ppm.
实施例2Example 2
采用自耗凝壳工艺熔炼高铌钛铝合金后制成直径为30mm，长度为150mm的圆棒铸坯，然后将铸坯的表面氧化皮去除，将铸坯加工成可以连接的直径为25mm长度为140mm的棒材；采用无坩埚感应加热连续惰性气体雾化工艺将棒材制成粉末，工艺参数为惰性气体压力3.0MPa，氩气流量200L s-1。所制备的粉末球形度达到93％，粉末收得率87％。当粒度为-200目时，合金粉中的氧含量为1200ppm。The high-niobium titanium-aluminum alloy is smelted by the consumable solidification process to make a round bar billet with a diameter of 30mm and a length of 150mm, and then the surface oxide skin of the billet is removed, and the billet is processed into a diameter of 25mm and a length that can be connected. It is a 140mm bar; the bar is made into powder by induction heating continuous inert gas atomization process without crucible, and the process parameters are inert gas pressure 3.0MPa, argon flow rate 200L s -1 . The sphericity of the prepared powder reaches 93%, and the powder yield is 87%. When the particle size is -200 mesh, the oxygen content in the alloy powder is 1200ppm.
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| CN111702183A (en) * | 2020-07-09 | 2020-09-25 | 四川容克斯科技有限公司 | Spherical titanium-aluminum alloy powder and preparation method and application thereof |
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| CN113684383A (en) * | 2020-05-19 | 2021-11-23 | 宝武特种冶金有限公司 | Preparation method of large-size high-Nb TiAl alloy ingot |
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2008
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| CN101812604A (en) * | 2009-06-09 | 2010-08-25 | 北京科技大学 | Method for improving long-term oxidation resistance of high-niobium titanium-aluminum alloy through adding yttrium at high temperature |
| CN101850424A (en) * | 2010-05-26 | 2010-10-06 | 北京科技大学 | A method for preparing a large amount of fine spherical titanium-aluminum-based alloy powder |
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| CN104625066A (en) * | 2015-01-30 | 2015-05-20 | 北京科技大学 | Method for manufacturing high-niobium titanium-aluminum alloy material by adopting two-step pressure infiltration |
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| CN107234245A (en) * | 2017-08-12 | 2017-10-10 | 长沙唯特冶金工程技术有限公司 | The equipment that a kind of use bar continuous feed produces spherical powder |
| CN107745130A (en) * | 2017-09-26 | 2018-03-02 | 江苏威拉里新材料科技有限公司 | A kind of high temperature niobium tungsten alloy raw powder's production technology |
| CN109877332A (en) * | 2019-04-16 | 2019-06-14 | 上海材料研究所 | A method for improving the fine powder rate of titanium or titanium alloy gas atomized powder |
| CN113684383A (en) * | 2020-05-19 | 2021-11-23 | 宝武特种冶金有限公司 | Preparation method of large-size high-Nb TiAl alloy ingot |
| CN113684383B (en) * | 2020-05-19 | 2022-10-18 | 宝武特种冶金有限公司 | Preparation method of large-size high-Nb TiAl alloy ingot |
| CN111702183A (en) * | 2020-07-09 | 2020-09-25 | 四川容克斯科技有限公司 | Spherical titanium-aluminum alloy powder and preparation method and application thereof |
| CN112756624A (en) * | 2020-12-11 | 2021-05-07 | 丹阳层现三维科技有限公司 | Method for reducing cracks in selective laser melting printing titanium-aluminum alloy |
| CN113210616A (en) * | 2021-05-11 | 2021-08-06 | 北京钢研高纳科技股份有限公司 | Ultra-fine Ti2AlNb alloy powder and preparation method and application thereof |
| CN113492213A (en) * | 2021-09-07 | 2021-10-12 | 西安欧中材料科技有限公司 | Preparation method and equipment of high-sphericity low-oxygen-content TiAl alloy powder |
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