CN110724885B - Preparation method of large-size light magnesium-aluminum-based amorphous alloy - Google Patents
Preparation method of large-size light magnesium-aluminum-based amorphous alloy Download PDFInfo
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- 229910000808 amorphous metal alloy Inorganic materials 0.000 title claims abstract description 175
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000011777 magnesium Substances 0.000 claims abstract description 72
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 69
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 69
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 67
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000012071 phase Substances 0.000 claims abstract description 66
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- 230000000996 additive effect Effects 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000011812 mixed powder Substances 0.000 claims abstract description 13
- 239000007791 liquid phase Substances 0.000 claims abstract description 7
- 239000013526 supercooled liquid Substances 0.000 claims description 22
- 238000000498 ball milling Methods 0.000 claims description 20
- 238000002425 crystallisation Methods 0.000 claims description 14
- 230000008025 crystallization Effects 0.000 claims description 14
- 239000011261 inert gas Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 10
- 238000002844 melting Methods 0.000 claims description 5
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000000889 atomisation Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
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- 229910001051 Magnalium Inorganic materials 0.000 claims 1
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- 239000000203 mixture Substances 0.000 abstract description 32
- 239000002131 composite material Substances 0.000 abstract description 7
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- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000009689 gas atomisation Methods 0.000 description 4
- 238000005728 strengthening Methods 0.000 description 4
- 238000003723 Smelting Methods 0.000 description 3
- 238000005266 casting Methods 0.000 description 3
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- 150000002739 metals Chemical class 0.000 description 3
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- 229910052786 argon Inorganic materials 0.000 description 2
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- 238000001816 cooling Methods 0.000 description 2
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- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000013528 artificial neural network Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
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- 229910052719 titanium Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C45/00—Amorphous alloys
- C22C45/005—Amorphous alloys with Mg as the major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
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Abstract
本发明属于非晶合金领域，更具体地，涉及一种大尺寸轻质镁铝基非晶合金的制备方法。按照目标合金成分比例称取粉末状的镁基非晶合金及铝基非晶合金，混合均匀获得镁铝基非晶合金混合粉末；镁基非晶合金及铝基非晶合金的成分的过冷液相区间有重叠；通过粉末烧结工艺或激光增材制造技术制备镁铝基非晶合金。本发明利用铝基非晶作为增韧相改善镁基非晶合金的室温塑性或者利用镁基非晶作为增强相提高铝基非晶的强度，采用粉末烧结工艺或激光增材制造技术制备获得大尺寸轻质高强镁铝基非晶合金，由此解决现有技术采用晶体第二相与非晶基体内部结构存在较大差异，变形模式相差较大，界面冶金结合实现困难，导致所制备的复合材料性能不高的技术问题。
The invention belongs to the field of amorphous alloys, and more particularly relates to a preparation method of a large-size lightweight magnesium-aluminum-based amorphous alloy. Weigh powdered magnesium-based amorphous alloy and aluminum-based amorphous alloy according to the target alloy composition ratio, and mix them uniformly to obtain a mixed powder of magnesium-aluminum-based amorphous alloy; The liquid phase interval overlaps; magnesium-aluminum-based amorphous alloys are prepared by powder sintering process or laser additive manufacturing technology. The invention uses aluminum-based amorphous as a toughening phase to improve the room temperature plasticity of magnesium-based amorphous alloys or uses magnesium-based amorphous as a reinforcing phase to improve the strength of aluminum-based amorphous, and adopts powder sintering process or laser additive manufacturing technology to prepare large alloys. The magnesium-aluminum-based amorphous alloy, which is light in size, light in weight and high in strength, solves the problem that the existing technology uses a large difference in the internal structure of the crystal second phase and the amorphous matrix, the deformation mode is quite different, and the interface metallurgical bonding is difficult to achieve, resulting in the prepared composite Technical problems with low material properties.
Description
技术领域technical field
本发明属于非晶合金领域，更具体地，涉及一种大尺寸轻质镁铝基非晶合金的制备方法。The invention belongs to the field of amorphous alloys, and more particularly relates to a preparation method of a large-size lightweight magnesium-aluminum-based amorphous alloy.
背景技术Background technique
新型轻质高强材料在航空航天、汽车轻量化、国防装备、大型跨海大桥、高层建筑等领域被广泛应用。钛、镁、铝三种金属以其储量丰富、密度低，强度性能好，是目前常用的轻质结构材料。镁基、铝基非晶合金的强度是传统的镁合金、铝合金材料的3～5倍，同时具有良好的耐腐蚀性、耐磨性、高温热塑性成形性，是一种极具应用前景的新型轻质高强结构材料。但是非晶合金制备需要较快的冷却速率，零件尺寸、形状受到极大限制，同时其室温塑性普遍较差，尤其是镁基非晶合金室温呈现完全脆性断裂，在实际服役过程中存在极大的安全隐患。铝基非晶合金室温塑性相对较好，但是其非晶形成能力较差，临界成形尺寸普遍小于1mm，成形难度大，应用困难。New lightweight and high-strength materials are widely used in aerospace, automotive lightweight, defense equipment, large-scale sea-crossing bridges, high-rise buildings and other fields. Titanium, magnesium and aluminum are widely used lightweight structural materials due to their abundant reserves, low density and good strength properties. The strength of magnesium-based and aluminum-based amorphous alloys is 3 to 5 times that of traditional magnesium alloys and aluminum alloys. At the same time, it has good corrosion resistance, wear resistance, and high temperature thermoplastic formability. It is a promising application. New lightweight high-strength structural material. However, the preparation of amorphous alloys requires a fast cooling rate, the size and shape of the parts are greatly limited, and their room temperature plasticity is generally poor. security risks. Aluminum-based amorphous alloys have relatively good room temperature plasticity, but their amorphous forming ability is poor, and the critical forming size is generally less than 1 mm, which is difficult to form and difficult to apply.
粉末烧结和增材制造能在一定程度上突破非晶合金构件制造尺寸、形状限制，同时目前一般采用高熔点陶瓷或金属等晶体材料作为第二相来达到对非晶基体增强或增韧的目的。晶体第二相与非晶基体内部结构存在较大差异，变形模式相差较大，界面冶金结合实现困难，导致所制备的复合材料性能不高。Powder sintering and additive manufacturing can break through the size and shape limitations of amorphous alloy components to a certain extent. At the same time, crystalline materials such as high melting point ceramics or metals are generally used as the second phase to achieve the purpose of strengthening or toughening the amorphous matrix. . There is a big difference in the internal structure of the crystalline second phase and the amorphous matrix, the deformation mode is quite different, and the interface metallurgical bonding is difficult to achieve, resulting in the low performance of the prepared composite material.
发明内容SUMMARY OF THE INVENTION
针对现有技术的以上缺陷或改进需求，本发明提供了一种大尺寸轻质镁铝基非晶合金的制备方法，其利用铝基非晶作为增韧相改善镁基非晶合金的室温塑性或者利用镁基非晶作为增强相提高铝基非晶的强度，采用粉末烧结工艺或激光增材制造技术制备获得大尺寸轻质高强镁铝基非晶合金，由此解决现有技术采用晶体第二相与非晶基体内部结构存在较大差异，变形模式相差较大，界面冶金结合实现困难，导致所制备的复合材料性能不高的技术问题。In view of the above defects or improvement needs of the prior art, the present invention provides a method for preparing a large-size lightweight magnesium-aluminum-based amorphous alloy, which uses aluminum-based amorphous as a toughening phase to improve the room temperature plasticity of the magnesium-based amorphous alloy Or use magnesium-based amorphous as a reinforcing phase to improve the strength of aluminum-based amorphous, and use powder sintering process or laser additive manufacturing technology to prepare large-size, lightweight, high-strength magnesium-aluminum-based amorphous alloys, thereby solving the problem of using crystal first in the prior art. There is a big difference between the internal structure of the two-phase and the amorphous matrix, the deformation mode is quite different, and the interface metallurgical bonding is difficult to achieve, which leads to the technical problem that the performance of the prepared composite material is not high.
为实现上述目的，按照本发明的一个方面，提供了一种镁铝基非晶合金的制备方法，包括如下步骤：In order to achieve the above object, according to one aspect of the present invention, a preparation method of a magnesium-aluminum-based amorphous alloy is provided, comprising the following steps:
(1)按照目标合金成分比例称取粉末状的镁基非晶合金及铝基非晶合金，混合均匀获得镁铝基非晶合金混合粉末；所述镁基非晶合金及铝基非晶合金的成分的过冷液相区间有重叠；(1) Weigh powdered magnesium-based amorphous alloy and aluminum-based amorphous alloy according to the target alloy composition ratio, and mix them uniformly to obtain a mixed powder of magnesium-aluminum-based amorphous alloy; the magnesium-based amorphous alloy and aluminum-based amorphous alloy The subcooled liquid phase range of the components overlaps;
(2)通过粉末烧结工艺或激光增材制造技术将所述镁铝基非晶合金混合粉末制备成镁铝基非晶合金。(2) The magnesium-aluminum-based amorphous alloy mixed powder is prepared into a magnesium-aluminum-based amorphous alloy by a powder sintering process or a laser additive manufacturing technology.
优选地，步骤(1)所述镁基非晶合金及铝基非晶合金的选择标准为：非晶合金成分临界成形尺寸不小于0.1mm，过冷液相温度区间的上限和下限的差值ΔTx大于20K，且热塑性成形能力指标S＞0.15。Preferably, the selection criteria of the magnesium-based amorphous alloy and the aluminum-based amorphous alloy in step (1) are: the critical forming size of the amorphous alloy composition is not less than 0.1 mm, the difference between the upper limit and the lower limit of the subcooled liquidus temperature range ΔT x is greater than 20K, and the thermoplastic formability index S>0.15.
优选地，所述镁基非晶合金及铝基非晶合金的成分的过冷液相区的重叠区间的上限和下限的差值不小于5K。Preferably, the difference between the upper limit and the lower limit of the overlapping interval of the supercooled liquid phase regions of the compositions of the magnesium-based amorphous alloy and the aluminum-based amorphous alloy is not less than 5K.
优选地，步骤(1)所述粉末状的所述镁基非晶合金及铝基非晶合金按照如下方法获得：采用气雾化法、机械球磨法、等离子球磨或等离子旋转电极法将所述镁基非晶合金及铝基非晶合金制备成粒径为微米级或纳米级的非晶合金粉末。Preferably, the powdered magnesium-based amorphous alloy and aluminum-based amorphous alloy in step (1) are obtained according to the following method: by gas atomization, mechanical ball milling, plasma ball milling or plasma rotating electrode method The magnesium-based amorphous alloy and the aluminum-based amorphous alloy are prepared into amorphous alloy powders with a particle size of micron or nanometer.
优选地，步骤(1)采用球磨将所述粉末状的镁基非晶合金及铝基非晶合金混合均匀；所述球磨过程的工艺参数为：磨球材质为硬质合金、不锈钢或玛瑙，转速为100～800r/min，球料比为30:1～3:1，球磨时间为10min～24h。Preferably, in step (1), the powdered magnesium-based amorphous alloy and the aluminum-based amorphous alloy are uniformly mixed by ball milling; the process parameters of the ball milling process are: the material of the grinding ball is cemented carbide, stainless steel or agate, The rotating speed is 100～800r/min, the ball-to-material ratio is 30:1～3:1, and the ball milling time is 10min～24h.
优选地，步骤(2)所述粉末烧结过程采用的温度处于所述镁基非晶合金和铝基非晶合金成分的过冷液相区的重叠区间之内，粉末烧结升温速率为10K/min～500K/min,粉末烧结压力为30MPa～5GPa，在真空度＜10Pa或在惰性气体保护环境中进行烧结，成形时间短于所述镁基非晶合金和铝基非晶合金成分在所采用的烧结温度下的最小晶化起始时间。Preferably, the temperature used in the powder sintering process in step (2) is within the overlapping range of the supercooled liquid phase regions of the magnesium-based amorphous alloy and aluminum-based amorphous alloy components, and the powder sintering heating rate is 10K/min ～500K/min, the powder sintering pressure is 30MPa～5GPa, the sintering is carried out in a vacuum degree <10Pa or in an inert gas protection environment, and the forming time is shorter than that of the magnesium-based amorphous alloy and aluminum-based amorphous alloy. Minimum crystallization onset time at sintering temperature.
优选地，步骤(3)所述粉末烧结过程采用的温度处于所述镁基非晶合金和铝基非晶合金成分的过冷液相区的重叠区间之内，且不低于所述重叠区间的中间温度值；所述镁铝基非晶合金混合粉末的粒径小于1um；粉末烧结升温速率为10K/min～500K/min,粉末烧结压力为大于1GPa，在真空度＜1×10-4Pa或在惰性气体保护环境中进行烧结，成形时间短于所述镁基非晶合金和铝基非晶合金成分在所采用的烧结温度下的最小晶化起始时间。Preferably, the temperature used in the powder sintering process in step (3) is within the overlapping interval of the supercooled liquid phase regions of the magnesium-based amorphous alloy and the aluminum-based amorphous alloy composition, and is not lower than the overlapping interval The particle size of the magnesium-aluminum-based amorphous alloy mixed powder is less than 1um; the heating rate of powder sintering is 10K/min～500K/min, the powder sintering pressure is greater than 1GPa, and the vacuum degree is less than 1×10 -4 Pa or sintering in an inert gas atmosphere, the forming time is shorter than the minimum crystallization initiation time of the magnesium-based amorphous alloy and aluminum-based amorphous alloy components at the adopted sintering temperature.
优选地，步骤(3)所述激光增材制造的工艺参数为：激光熔池温度处于所述镁基非晶合金和铝基非晶合金成分的过冷液相区的重叠区间之内，激光功率500W～20000W，扫描速度60mm/min～3000mm/min，激光光斑直径0.1mm～5mm，在真空度小于10Pa或在惰性气体保护环境中进行增材制造；成形时间短于所述镁基非晶合金和铝基非晶合金成分在所采用的烧结温度下的最小晶化起始时间。Preferably, the process parameters of the laser additive manufacturing in step (3) are: the temperature of the laser molten pool is within the overlapping range of the supercooled liquid phase regions of the magnesium-based amorphous alloy and the aluminum-based amorphous alloy composition, and the laser Power 500W~20000W, scanning speed 60mm/min~3000mm/min, laser spot diameter 0.1mm~5mm, additive manufacturing under vacuum less than 10Pa or inert gas protection environment; forming time is shorter than the magnesium-based amorphous Minimum crystallization onset time for alloys and Al-based amorphous alloy compositions at the sintering temperature employed.
优选地，步骤(3)所述激光增材制造的工艺参数为：激光熔池温度处于所述镁基非晶合金和铝基非晶合金成分的过冷液相区的重叠区间之内，且不低于所述重叠区间的中间温度值；激光功率500W～20000W，扫描速度60mm/min～3000mm/min，激光光斑直径0.1mm～0.5mm，在真空度小于1×10-4Pa或在惰性气体保护环境中进行增材制造；所述镁铝基非晶合金混合粉末的粒径小于1um；成形时间短于所述镁基非晶合金和铝基非晶合金成分在所采用的烧结温度下的最小晶化起始时间。Preferably, the process parameters of the laser additive manufacturing in step (3) are: the temperature of the laser molten pool is within the overlapping range of the supercooled liquid phase regions of the magnesium-based amorphous alloy and the aluminum-based amorphous alloy composition, and Not lower than the middle temperature value of the overlapping interval; laser power 500W～20000W, scanning speed 60mm/min～3000mm/min, laser spot diameter 0.1mm～0.5mm, vacuum degree less than 1×10 -4 Pa or inert Additive manufacturing is performed in a gas protection environment; the particle size of the magnesium-aluminum-based amorphous alloy mixed powder is less than 1um; the forming time is shorter than the sintering temperature used for the magnesium-based amorphous alloy and aluminum-based amorphous alloy components minimum crystallization onset time.
总体而言，通过本发明所构思的以上技术方案与现有技术相比，能够取得下列有益效果：In general, compared with the prior art, the above technical solutions conceived by the present invention can achieve the following beneficial effects:
(1)本发明针对镁基、铝基非晶合金各自的特点，提出了一种镁铝基双相非晶复合材料的制备方法，利用铝基非晶作为增韧相改善镁基非晶合金的室温塑性或者利用镁基非晶作为增强相提高铝基非晶的强度。相比于传统采用高熔点陶瓷或金属等晶体材料作为第二相的方式，双相非晶两相之间结构相同，变形机制类似，变形协调性较好，且成形时两相均处于过冷液相区，粘度较低，原子扩散、运动能力强，界面结合强度高，能够达到更好的增强/增韧效果。同时，该发明能够通过调整镁、铝比例，实现轻质镁铝基非晶合金的成分灵活设计、制备。(1) Aiming at the respective characteristics of magnesium-based and aluminum-based amorphous alloys, the present invention proposes a preparation method of a magnesium-aluminum-based dual-phase amorphous composite material, and uses aluminum-based amorphous as a toughening phase to improve magnesium-based amorphous alloys. room temperature plasticity or using magnesium-based amorphous as a reinforcing phase to improve the strength of aluminum-based amorphous. Compared with the traditional method of using crystalline materials such as high-melting point ceramics or metals as the second phase, the structure of the two-phase amorphous phase is the same, the deformation mechanism is similar, and the deformation coordination is better, and both phases are supercooled during forming. In the liquid phase region, the viscosity is low, the atomic diffusion and movement ability is strong, and the interface bonding strength is high, which can achieve better strengthening/toughening effect. At the same time, the invention can realize the flexible design and preparation of the composition of the lightweight magnesium-aluminum-based amorphous alloy by adjusting the ratio of magnesium and aluminum.
(2)本发明通过控制粉末烧结工艺参数或激光增材制造工艺参数，能够获得单相镁铝基非晶复合材料，因此本发明提出了一种新型的非晶合金成分设计与制备方法，具体为利用粉末烧结过程中原子扩散均匀化效应及非晶合金在过冷液相区的超塑性实现两种非晶合金成分的充分揉和，制备具有单一非晶相的镁铝基非晶合金。相比于传统的非晶合金成分研发方式，本方法能够实现非晶合金成分的灵活设计、制备、成形一体化，同时利用粉末烧结或增材制造技术解决非晶合金制备的尺寸、形状限制难题，避免了镁铝基非晶熔炼时由于镁极易挥发、氧化导致的成分改变和安全隐患问题。(2) The present invention can obtain a single-phase magnesium-aluminum-based amorphous composite material by controlling the powder sintering process parameters or the laser additive manufacturing process parameters. Therefore, the present invention proposes a new type of amorphous alloy composition design and preparation method, specifically A magnesium-aluminum-based amorphous alloy with a single amorphous phase was prepared in order to utilize the atomic diffusion homogenization effect in the powder sintering process and the superplasticity of the amorphous alloy in the supercooled liquid phase region to achieve sufficient mixing of the two amorphous alloy components. Compared with the traditional research and development methods of amorphous alloy components, this method can realize the flexible design, preparation, and integration of amorphous alloy components, and at the same time use powder sintering or additive manufacturing technology to solve the size and shape limitations of amorphous alloy preparation. , to avoid the composition change and safety hazards caused by the extremely volatile and oxidation of magnesium during magnesium-aluminum-based amorphous smelting.
附图说明Description of drawings
图1是本发明的一种大尺寸轻质镁铝基非晶合金及其制备方法的流程图。Fig. 1 is a flow chart of a large-size light-weight magnesium-aluminum-based amorphous alloy and a preparation method thereof of the present invention.
具体实施方式Detailed ways
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。此外，下面所描述的本发明各个实施方式中所涉及到的技术特征只要彼此之间未构成冲突就可以相互组合。In order to make the objectives, technical solutions and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention, but not to limit the present invention. In addition, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.
针对镁基、铝基非晶合金的应用瓶颈和新型轻质高强结构材料的制造需求，本发明提供了一种大尺寸轻质镁铝基非晶合金的制备方法，该方法可以实现镁铝基非晶合金的成分灵活设计、制备，通过调整镁、铝比例，获得大尺寸轻质高强单相或双相镁铝基块体非晶合金。Aiming at the application bottleneck of magnesium-based and aluminum-based amorphous alloys and the manufacturing requirements of new lightweight and high-strength structural materials, the present invention provides a preparation method of large-size lightweight magnesium-aluminum-based amorphous alloys, which can realize magnesium-aluminum-based amorphous alloys. The composition of the amorphous alloy is flexibly designed and prepared. By adjusting the ratio of magnesium and aluminum, a large-size, light-weight, high-strength single-phase or dual-phase magnesium-aluminum-based bulk amorphous alloy can be obtained.
本发明提供的一种镁铝基非晶合金的制备方法，如图1所示，包括如下步骤：The preparation method of a magnesium-aluminum-based amorphous alloy provided by the present invention, as shown in Figure 1, includes the following steps:
(1)按照目标合金成分比例称取粉末状的镁基非晶合金及铝基非晶合金，混合均匀获得镁铝基非晶合金混合粉末；所述镁基非晶合金及铝基非晶合金的成分的过冷液相区间有重叠；(1) Weigh powdered magnesium-based amorphous alloy and aluminum-based amorphous alloy according to the target alloy composition ratio, and mix them uniformly to obtain a mixed powder of magnesium-aluminum-based amorphous alloy; the magnesium-based amorphous alloy and aluminum-based amorphous alloy The subcooled liquid phase range of the components overlaps;
(2)通过粉末烧结工艺或激光增材制造技术将所述镁铝基非晶合金混合粉末制备成镁铝基非晶合金。(2) The magnesium-aluminum-based amorphous alloy mixed powder is prepared into a magnesium-aluminum-based amorphous alloy by a powder sintering process or a laser additive manufacturing technology.
根据目标非晶合金性能要求，为了获得非晶形成能力较强的镁铝基非晶合金，一些实施例中，步骤(1)所述镁基非晶合金及铝基非晶合金的选择标准为：非晶合金成分临界成形尺寸不小于0.1mm，过冷液相温度区间的上限和下限的差值ΔTx大于20K，且热塑性成形能力指标S＞0.15。所述过冷液相温度区间是由非晶合金的晶化起始温度Tx与玻璃转变温度Tg形成的温度区间，其中晶化起始温度Tx作为该区间的上限，玻璃转变温度Tg作为该区间的下限。非晶成分的选择可以采用理论判据法、高通量实验法、元素替代法、机器学习及神经网络预测等方法。According to the performance requirements of the target amorphous alloy, in order to obtain a magnesium-aluminum-based amorphous alloy with strong amorphous forming ability, in some embodiments, the selection criteria of the magnesium-based amorphous alloy and the aluminum-based amorphous alloy in step (1) are: : The critical forming dimension of the amorphous alloy composition is not less than 0.1mm, the difference ΔT x between the upper limit and the lower limit of the subcooled liquidus temperature range is greater than 20K, and the thermoplastic formability index S>0.15. The supercooled liquidus temperature interval is a temperature interval formed by the crystallization initiation temperature T x of the amorphous alloy and the glass transition temperature T g , wherein the crystallization initiation temperature T x is the upper limit of this interval, and the glass transition temperature T g as the lower limit of the interval. The selection of amorphous components can adopt methods such as theoretical criterion method, high-throughput experiment method, element substitution method, machine learning and neural network prediction.
本发明两种基体非晶合金成分的过冷液相区应有一定程度的重叠，一些优选实施例中，本发明所述镁基非晶合金及铝基非晶合金的成分的过冷液相区的重叠区间上下限的差值不小于5K。The supercooled liquid phase regions of the two base amorphous alloy compositions of the present invention should overlap to a certain extent. In some preferred embodiments, the supercooled liquid phase regions of the compositions of the magnesium-based amorphous alloy and aluminum-based amorphous alloy of the present invention The difference between the upper and lower limits of the overlapping interval of the zones shall not be less than 5K.
本发明步骤(1)可以采用粉末制备技术获得微米级或纳米级的镁基和铝基非晶合金粉末。一些实施例中，步骤(1)采用气雾化法、机械球磨法、等离子球磨或等离子旋转电极法将所述镁基非晶合金及铝基非晶合金制备成粒径为微米级或纳米级的非晶合金粉末。In step (1) of the present invention, powder preparation technology can be used to obtain micron-scale or nano-scale magnesium-based and aluminum-based amorphous alloy powders. In some embodiments, step (1) adopts gas atomization method, mechanical ball milling method, plasma ball milling or plasma rotating electrode method to prepare the magnesium-based amorphous alloy and aluminum-based amorphous alloy into a micron-scale or nano-scale particle size. amorphous alloy powder.
步骤(2)可以采用各种粉末混合的方法将镁基非晶合金粉末及铝基非晶合金粉末混合均匀。一些实施例中，步骤(2)采用球磨工艺进行两种粉末的混合。其中所述球磨过程的工艺参数为：磨球材质为硬质合金、不锈钢或玛瑙，转速为100～800r/min，球料比为30:1～3:1，球磨时间为10min～24h。In step (2), various powder mixing methods can be used to mix the magnesium-based amorphous alloy powder and the aluminum-based amorphous alloy powder uniformly. In some embodiments, step (2) uses a ball milling process to mix the two powders. The process parameters of the ball milling process are as follows: the material of the grinding ball is cemented carbide, stainless steel or agate, the rotational speed is 100-800 r/min, the ball-to-material ratio is 30:1-3:1, and the ball-milling time is 10min-24h.
一些实施例中，为了获得大尺寸轻质高强镁铝基双相或单相块体非晶，步骤(3)所述粉末烧结过程采用的温度处于所述镁基非晶合金和铝基非晶合金成分的过冷液相区的重叠区间之内，粉末烧结升温速率为10K/min～500K/min,粉末烧结压力为30MPa～5GPa，真空度＜10Pa或在惰性气体保护环境中进行，成形时间短于所述镁基非晶合金和铝基非晶合金成分在所采用的烧结温度下的最小晶化起始时间。In some embodiments, in order to obtain large-sized, light-weight, high-strength magnesium-aluminum-based dual-phase or single-phase bulk amorphous, the temperature used in the powder sintering process in step (3) is at the temperature of the magnesium-based amorphous alloy and the aluminum-based amorphous alloy. Within the overlapping range of the supercooled liquid phase region of the alloy composition, the heating rate of powder sintering is 10K/min～500K/min, the powder sintering pressure is 30MPa～5GPa, the vacuum degree is less than 10Pa or carried out in an inert gas protection environment, and the forming time is Shorter than the minimum crystallization onset time of the magnesium-based amorphous alloy and aluminum-based amorphous alloy components at the sintering temperature employed.
另一些实施例中，为了获得具有单一非晶相的镁铝基非晶合金，可通过控制粉末烧结工艺参数确保两种非晶合金成分的均匀混合与分布。比如一些实施例中，步骤(3)通过控制所述粉末烧结过程采用的温度处于所述镁基非晶合金和铝基非晶合金成分的过冷液相区的重叠区间之内，且不低于所述重叠区间的中间温度值；所述镁铝基非晶合金混合粉末的粒径小于1um；粉末烧结升温速率为10K/min～500K/min,粉末烧结压力为大于1GPa，真空度＜1×10-4Pa或在惰性气体保护环境中进行，成形时间短于所述镁基非晶合金和铝基非晶合金成分在所采用的烧结温度下的最小晶化起始时间，而得到单一非晶相镁铝基非晶合金。In other embodiments, in order to obtain a magnesium-aluminum-based amorphous alloy with a single amorphous phase, the powder sintering process parameters can be controlled to ensure uniform mixing and distribution of the two amorphous alloy components. For example, in some embodiments, the temperature used in the powder sintering process in step (3) is within the overlapping range of the supercooled liquid phase regions of the magnesium-based amorphous alloy and the aluminum-based amorphous alloy composition, and is not lower than The temperature value in the middle of the overlapping interval; the particle size of the magnesium-aluminum-based amorphous alloy mixed powder is less than 1um; the powder sintering heating rate is 10K/min～500K/min, the powder sintering pressure is greater than 1GPa, and the vacuum degree is less than 1 ×10 -4 Pa or in an inert gas protective environment, the forming time is shorter than the minimum crystallization initiation time of the magnesium-based amorphous alloy and aluminum-based amorphous alloy components at the adopted sintering temperature, and a single Amorphous magnesium-aluminum-based amorphous alloy.
一些实施例中，为了获得大尺寸轻质高强镁铝基双相或单相块体非晶，步骤(3)所述激光增材制造的工艺参数为：激光熔池温度处于所述镁基非晶合金和铝基非晶合金成分的过冷液相区的重叠区间之内，激光功率500W～20000W，扫描速度60mm/min～3000mm/min，激光光斑直径0.1mm～5mm，真空度小于10Pa或在惰性气体保护环境中进行；成形时间短于所述镁基非晶合金和铝基非晶合金成分在所采用的烧结温度下的最小晶化起始时间。In some embodiments, in order to obtain large-size, light-weight and high-strength magnesium-aluminum-based dual-phase or single-phase bulk amorphous, the process parameters of the laser additive manufacturing in step (3) are: Within the overlapping area of the supercooled liquid phase of crystalline alloy and aluminum-based amorphous alloy composition, the laser power is 500W~20000W, the scanning speed is 60mm/min~3000mm/min, the laser spot diameter is 0.1mm~5mm, and the vacuum degree is less than 10Pa or In an inert gas atmosphere; the forming time is shorter than the minimum crystallization initiation time of the magnesium-based amorphous alloy and aluminum-based amorphous alloy components at the sintering temperature employed.
另一些实施例中，为了获得具有单一非晶相的镁铝基非晶合金，可通过控制激光增材制造工艺参数确保两种非晶合金成分的均匀混合与分布。比如一些实施例中，步骤(3)所述激光增材制造的工艺参数为：激光熔池温度处于所述镁基非晶合金和铝基非晶合金成分的过冷液相区的重叠区间之内，且不低于所述重叠区间的中间温度值；激光功率500W～20000W，扫描速度60mm/min～3000mm/min，激光光斑直径0.1mm～0.5mm，真空度小于1×10- 4Pa或在惰性气体保护环境中进行；所述镁铝基非晶合金混合粉末的粒径小于1um；成形时间短于所述镁基非晶合金和铝基非晶合金成分在所采用的烧结温度下的最小晶化起始时间，而得到单一非晶相镁铝基非晶合金。In other embodiments, in order to obtain a magnesium-aluminum-based amorphous alloy with a single amorphous phase, the laser additive manufacturing process parameters can be controlled to ensure uniform mixing and distribution of the two amorphous alloy components. For example, in some embodiments, the process parameter of the laser additive manufacturing in step (3) is: the temperature of the laser molten pool is within the overlapping range of the supercooled liquid phase regions of the magnesium-based amorphous alloy and the aluminum-based amorphous alloy composition. within the range, and not lower than the middle temperature value of the overlap interval; laser power 500W～20000W, scanning speed 60mm/min～3000mm/min, laser spot diameter 0.1mm～0.5mm, vacuum degree less than 1×10 - 4 Pa or It is carried out in an inert gas protection environment; the particle size of the magnesium-aluminum-based amorphous alloy mixed powder is less than 1 μm; the forming time is shorter than the sintering temperature of the magnesium-based amorphous alloy and aluminum-based amorphous alloy components. The minimum crystallization initiation time, and a single amorphous phase magnesium-aluminum-based amorphous alloy is obtained.
本发明所述镁铝基单相块体非晶合金是指以镁、铝为主要合金组元、具有单一非晶相的合金体系，合金内部成分均匀，不存在宏观元素成分浓度差异。The magnesium-aluminum-based single-phase bulk amorphous alloy in the present invention refers to an alloy system with magnesium and aluminum as the main alloy components and a single amorphous phase.
本发明所述镁铝基双相块体非晶合金是指以其中一种成分为基体，另一成分为增强相或增韧相的复合材料，具有两种特征非晶衍射峰。The magnesium-aluminum-based dual-phase bulk amorphous alloy in the present invention refers to a composite material with one of the components as the matrix and the other as the reinforcing phase or toughening phase, and has two characteristic amorphous diffraction peaks.
采用本发明的镁铝非晶合金的制备方法，利用铝基非晶作为增韧相改善镁基非晶合金的室温塑性或者利用镁基非晶作为增强相提高铝基非晶的强度。相比于传统采用高熔点陶瓷或金属等晶体材料作为第二相的方式，双相非晶两相之间结构相同，变形机制类似，变形协调性较好，且成形时两相均处于过冷液相区，粘度较低，原子扩散、运动能力强，界面结合强度高，能够达到更好的增强/增韧效果。Using the preparation method of the magnesium-aluminum amorphous alloy of the present invention, the room temperature plasticity of the magnesium-based amorphous alloy is improved by using the aluminum-based amorphous as the toughening phase, or the strength of the aluminum-based amorphous alloy is improved by using the magnesium-based amorphous as the strengthening phase. Compared with the traditional method of using crystalline materials such as high-melting point ceramics or metals as the second phase, the structure of the two-phase amorphous phase is the same, the deformation mechanism is similar, and the deformation coordination is better, and both phases are supercooled during forming. In the liquid phase region, the viscosity is low, the atomic diffusion and movement ability is strong, and the interface bonding strength is high, which can achieve better strengthening/toughening effect.
另一方面，通过控制粉末烧结工艺或激光增材制造工艺的参数，利用粉末烧结过程或激光增材制造过程中原子扩散均匀化效应及非晶合金在过冷液相区的超塑性实现两种非晶合金成分的充分揉和，制备具有单一非晶相的镁铝基非晶合金。因此本发明提供的镁铝非晶合金的制备方法，在一定程度上也可以看作为一种新型的非晶合金成分设计与制备方法。根据需要可以获得任意目标成分的镁铝基非晶合金。On the other hand, by controlling the parameters of the powder sintering process or the laser additive manufacturing process, the atomic diffusion homogenization effect in the powder sintering process or the laser additive manufacturing process and the superplasticity of the amorphous alloy in the supercooled liquid phase region are used to achieve two kinds of The components of the amorphous alloy are fully kneaded to prepare a magnesium-aluminum-based amorphous alloy with a single amorphous phase. Therefore, the preparation method of the magnesium-aluminum amorphous alloy provided by the present invention can also be regarded as a novel composition design and preparation method of the amorphous alloy to a certain extent. A magnesium-aluminum-based amorphous alloy of any target composition can be obtained as required.
相比于传统的非晶合金成分研发方式，本方法能够实现非晶合金成分的灵活设计、制备、成形一体化，同时利用粉末烧结或增材制造技术解决非晶合金制备的尺寸、形状限制难题，避免了镁铝基非晶熔炼时由于镁极易挥发、氧化导致的成分改变和安全隐患问题。Compared with the traditional research and development methods of amorphous alloy components, this method can realize the flexible design, preparation, and integration of amorphous alloy components, and at the same time use powder sintering or additive manufacturing technology to solve the size and shape limitations of amorphous alloy preparation. , to avoid the composition change and safety hazards caused by the extremely volatile and oxidation of magnesium during magnesium-aluminum-based amorphous smelting.
目前采用传统的铸造方法制备块体Pd基非晶，其最大仅能制备得到约80mm直径的圆柱。另外镁基和铝基非晶合金非晶形成能力不是很好，采用铸造法直接急冷很难超过10mm(圆柱棒)。采用本发明提出的镁铝基单/双相非晶合金制备方法，在选择非晶形成能力较强的镁基、铝基非晶合金成分的基础上，利用粉末烧结或增材制造技术可以突破传统铸造方法制备镁铝基非晶合金的尺寸，比如本发明一些实施例中获得的镁铝基单/双相非晶合金的三维尺寸中任意两个尺寸大于10mm。At present, the traditional casting method is used to prepare bulk Pd-based amorphous, which can only prepare cylinders with a diameter of about 80 mm at the maximum. In addition, the amorphous forming ability of magnesium-based and aluminum-based amorphous alloys is not very good, and it is difficult to exceed 10mm (cylindrical rod) by direct quenching by casting method. Using the preparation method of magnesium-aluminum-based single/dual-phase amorphous alloy proposed by the present invention, on the basis of selecting magnesium-based and aluminum-based amorphous alloy components with strong amorphous forming ability, powder sintering or additive manufacturing technology can be used to make breakthroughs The size of the magnesium-aluminum-based amorphous alloy prepared by traditional casting methods, for example, any two of the three-dimensional dimensions of the magnesium-aluminum-based single/dual-phase amorphous alloy obtained in some embodiments of the present invention are greater than 10 mm.
针对新型轻质高强结构材料的应用需求，本发明提出一种镁铝基单/双相非晶合金制备方法，同时提供了一种非晶合金成分设计新方法。该方法首先优选出非晶形成能力较强的镁基、铝基非晶合金成分，制备粒径为微米级或纳米级的非晶粉末，按照最终合金成分比例称取粉末、球磨混合均匀后通过粉末烧结获得高致密块体非晶。通过优化烧结工艺参数，利用烧结过程中原子扩散均匀化效应以及非晶合金在过冷液相区的超塑性，获得性能良好的镁铝基双非晶相复合或单相非晶材料。该方法可以通过调整镁、铝比例，实现镁铝基非晶合金的成分灵活设计、制备，同时解决了镁铝基非晶合金制备熔炼时镁极易挥发、氧化等难题。Aiming at the application requirements of novel lightweight and high-strength structural materials, the present invention proposes a preparation method of magnesium-aluminum-based single/dual-phase amorphous alloy, and also provides a new method for designing amorphous alloy composition. The method first selects magnesium-based and aluminum-based amorphous alloy components with strong amorphous forming ability, prepares amorphous powder with a particle size of micrometer or nanometer, weighs the powder according to the proportion of the final alloy components, and mixes them uniformly by ball milling. Powder sintering to obtain highly dense bulk amorphous. By optimizing the sintering process parameters, utilizing the homogenization effect of atomic diffusion in the sintering process and the superplasticity of the amorphous alloy in the supercooled liquid phase region, a magnesium-aluminum-based double-amorphous phase composite or single-phase amorphous material with good performance is obtained. The method can realize the flexible design and preparation of the composition of the magnesium-aluminum-based amorphous alloy by adjusting the ratio of magnesium and aluminum, and at the same time solve the problems that magnesium is extremely volatile and oxidized when the magnesium-aluminum-based amorphous alloy is prepared and smelted.
以下为实施例：The following are examples:
在已开发的非晶合金成分库中优选出非晶形成能力较强的Mg54Cu28Ag7Y11镁基非晶合金、Al87Ni3Y10铝基非晶合金，其各项热物性参数如表1所示。Mg54Cu28Ag7Y11非晶合金非晶形成能力较强，过冷液相温度区间达到70K，Al87Ni3Y10非晶合金过冷液相区28K，室温断裂强度达到1140MPa，且两种非晶合金的过冷液相区重叠温度区间达到10K。In the developed amorphous alloy composition library, Mg 54 Cu 28 Ag 7 Y 11 magnesium-based amorphous alloy and Al 87 Ni 3 Y 10 aluminum-based amorphous alloy with strong amorphous forming ability are selected. The parameters are shown in Table 1. Mg 54 Cu 28 Ag 7 Y 11 amorphous alloy has strong amorphous forming ability, the subcooled liquid phase temperature range reaches 70K, Al 87 Ni 3 Y 10 amorphous alloy supercooled liquid phase zone is 28K, and the room temperature fracture strength reaches 1140MPa, and The overlapping temperature range of the supercooled liquid phase region of the two amorphous alloys reaches 10K.
表1两种非晶合金成分的热物性参数Table 1 Thermophysical parameters of two amorphous alloy compositions
按照名义成分称取高纯金属原料，利用气雾化技术制备筛选粒径范围为100nm～10um的镁基、铝基非晶合金粉末，具体工艺参数为：合金过热度为50～100℃，熔炼重复三次后得到母合金锭，高纯氩气雾化压力3.3MPa，导流孔直径为2mm。球磨混合均匀后采用热压烧结制备镁铝基单/双相块体非晶合金，球磨工艺参数为硬质合金磨球、转速300r/min，球料比10：1，球磨时间为2h，热压烧结工艺参数为：温度495K，压力600MPa、时间5min，升温速率20K/min，真空度5×10-3Pa。模具水冷快速冷却后获得块体非晶材料。Weigh high-purity metal raw materials according to the nominal composition, and use gas atomization technology to prepare magnesium-based and aluminum-based amorphous alloy powders with a particle size range of 100nm to 10um. After repeating three times, a master alloy ingot was obtained, the atomization pressure of high-purity argon gas was 3.3 MPa, and the diameter of the guide hole was 2 mm. The magnesium-aluminum-based single/dual-phase bulk amorphous alloy was prepared by hot pressing and sintering after ball milling evenly. The pressure sintering process parameters are: temperature 495K, pressure 600MPa, time 5min, heating rate 20K/min, vacuum degree 5×10 -3 Pa. The bulk amorphous material is obtained after the mold is rapidly cooled by water cooling.
当将具体工艺参数控制为：按照名义成分称取高纯金属原料，利用气雾化技术制备筛选粒径小于1um的镁基、铝基非晶合金粉末，具体工艺参数为合金过热度50～100℃，熔炼重复三次后得到母合金锭，高纯氩气雾化压力3.3MPa，导流孔直径1mm。球磨混合均匀后采用热压烧结制备镁铝基块体非晶合金，球磨工艺参数为硬质合金磨球、转速300r/min，球料比10：1，球磨时间为2h，热压烧结工艺参数为：温度498K，压力2.5GPa、时间5min，升温速率50K/min，真空度5×10-3Pa，可获得单相块体非晶材料。When the specific process parameters are controlled as follows: Weigh high-purity metal raw materials according to the nominal composition, and use gas atomization technology to prepare and screen magnesium-based and aluminum-based amorphous alloy powders with a particle size of less than 1um. The specific process parameters are alloy superheat 50 ~ 100 ℃, after the smelting is repeated three times, the master alloy ingot is obtained, the atomization pressure of high-purity argon gas is 3.3MPa, and the diameter of the guide hole is 1mm. After the ball milling is evenly mixed, the magnesium-aluminum-based bulk amorphous alloy is prepared by hot-pressing sintering. The ball-milling process parameters are cemented carbide grinding balls, rotating speed 300r/min, ball-to-material ratio 10:1, ball milling time 2h, hot-pressing sintering process parameters It is: temperature 498K, pressure 2.5GPa, time 5min, heating rate 50K/min, vacuum degree 5×10 -3 Pa, single-phase bulk amorphous material can be obtained.
本领域的技术人员容易理解，以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。Those skilled in the art can easily understand that the above are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention, etc., All should be included within the protection scope of the present invention.
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