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CN104789804A - Method for preparing titanium alloy granule reinforced magnesium-based composite material - Google Patents

Method for preparing titanium alloy granule reinforced magnesium-based composite material Download PDF

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CN104789804A
CN104789804A CN201510140995.6A CN201510140995A CN104789804A CN 104789804 A CN104789804 A CN 104789804A CN 201510140995 A CN201510140995 A CN 201510140995A CN 104789804 A CN104789804 A CN 104789804A
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magnesium
titanium alloy
composite material
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CN104789804B (en
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王晓军
王晓明
胡小石
吴昆�
郑明毅
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Jiaxing Bincheng Iot Technology Co ltd
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Harbin Institute of Technology Shenzhen
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Abstract

一种钛合金颗粒增强镁基复合材料的制备方法,它涉及一种镁基复合材料的制备方法。本发明是要解决目前的镁基复合材料还无法同时具备强度较高和塑性较好的技术问题。本发明的制备方法为:(1)制备半固态熔融镁合金;(2)制备钛合金颗粒-镁合金混合熔体;(3)制备钛合金颗粒增强镁基复合材料。本发明采用TC4(Ti-6Al-4V)钛合金颗粒作为镁合金的增强体,通过搅拌铸造方法以及控制钛合金颗粒的体积分数和颗粒尺寸大小,所制得的复合材料具有强度高和塑韧性好兼备的优异力学性能,与同体积分数同颗粒尺寸的常见陶瓷颗粒增强体制备的镁基复合材料相比,强度相差不大,而塑性明显好于后者。本发明主要应用于制备镁基复合材料。

The invention discloses a preparation method of a titanium alloy particle reinforced magnesium-based composite material, which relates to a preparation method of a magnesium-based composite material. The invention aims to solve the technical problem that the current magnesium-based composite materials cannot simultaneously have high strength and good plasticity. The preparation method of the invention includes: (1) preparing semi-solid molten magnesium alloy; (2) preparing titanium alloy particle-magnesium alloy mixed melt; (3) preparing titanium alloy particle-reinforced magnesium-based composite material. The present invention adopts TC4 (Ti-6Al-4V) titanium alloy particles as the reinforcing body of magnesium alloy, and through the stirring casting method and controlling the volume fraction and particle size of titanium alloy particles, the prepared composite material has high strength and plastic toughness Compared with magnesium-based composites prepared by common ceramic particle reinforcements with the same volume fraction and particle size, the strength is not much different, and the plasticity is obviously better than the latter. The invention is mainly applied to the preparation of magnesium-based composite materials.

Description

一种钛合金颗粒增强镁基复合材料的制备方法A kind of preparation method of titanium alloy particle reinforced magnesium matrix composite material

技术领域technical field

本发明涉及一种镁基复合材料的制备方法。The invention relates to a preparation method of a magnesium-based composite material.

背景技术Background technique

目前普遍采用陶瓷颗粒作为镁基复合材料的增强体,如SiC、B4C、TiC、TiC、Al2O3、Y2O3、TiO2、Mg2Si等,这主要是因为陶瓷具有极高的强度、刚度、杨氏模量和较好的稳定性,但是以其增强的复合材料在提高材料强度的同时,塑性远低于基体材料,这一问题限制了镁基复合材料更为广泛的应用。At present, ceramic particles are generally used as reinforcements of magnesium-based composites, such as SiC, B 4 C, TiC, TiC, Al 2 O 3 , Y 2 O 3 , TiO 2 , Mg 2 Si, etc., mainly because ceramics have extremely High strength, stiffness, Young's modulus and good stability, but the plasticity of the reinforced composite material is much lower than that of the matrix material while increasing the strength of the material. This problem limits the wider use of magnesium-based composite materials. Applications.

钛具有强度高、塑韧性好、耐蚀性好、耐热性高等特点,钛的密度较小,并且钛是比强度最高的金属,与常见陶瓷颗粒增强体相比,钛具有最大的优势是钛与镁之间的物理化学性质相似,兼容性很好,并且钛和镁之间的润湿性特别好,将常见的TC4钛合金颗粒加入到镁合金中,有望可以得到强度高和塑韧性好兼顾的镁基复合材料。现有方法主要局限于粉末冶金的制备方法,通过粉末冶金法制备的复合材料,其基体与颗粒之间的界面结合是通过热压烧结使固相基体颗粒和固相增强体颗粒结合起来的,这种通过固相与固相结合制备出的复合材料,其界面结合通常较差。另外,由于TC4钛合金颗粒的密度要比镁合金稍大些,所以当长时间静置钛合金颗粒-镁合金熔体时,就会发生颗粒沉积的现象,引起颗粒分布不均匀的问题。Titanium has the characteristics of high strength, good plastic toughness, good corrosion resistance, and high heat resistance. Titanium has a low density, and titanium is the metal with the highest specific strength. Compared with common ceramic particle reinforcements, titanium has the biggest advantage. The physical and chemical properties between titanium and magnesium are similar, the compatibility is very good, and the wettability between titanium and magnesium is particularly good. Adding common TC4 titanium alloy particles to magnesium alloys is expected to obtain high strength and toughness. A well-balanced magnesium-based composite material. Existing methods are mainly limited to the preparation method of powder metallurgy. The composite material prepared by powder metallurgy method, the interface between the matrix and the particles is combined by hot pressing and sintering to combine the solid phase matrix particles and the solid phase reinforcement particles. The interfacial bonding of such composite materials prepared by combining solid phases with solid phases is usually poor. In addition, since the density of TC4 titanium alloy particles is slightly larger than that of magnesium alloy, when the titanium alloy particles-magnesium alloy melt is left standing for a long time, the phenomenon of particle deposition will occur, causing the problem of uneven particle distribution.

发明内容Contents of the invention

本发明是要解决目前的镁基复合材料还无法同时具备强度较高和塑性较好的技术问题,从而提供一种钛合金颗粒增强镁基复合材料的制备方法。The present invention aims to solve the technical problem that current magnesium-based composite materials cannot simultaneously have high strength and good plasticity, thereby providing a preparation method of magnesium-based composite materials reinforced with titanium alloy particles.

本发明的钛合金颗粒增强镁基复合材料的制备方法按以下步骤进行:The preparation method of the titanium alloy particle reinforced magnesium-based composite material of the present invention is carried out according to the following steps:

一、制备半固态熔融镁合金:将基体镁合金升温至700℃~750℃,待基体合金完全熔化后将温度降至560℃~600℃,得到半固态熔融镁合金;1. Preparation of semi-solid molten magnesium alloy: raising the temperature of the matrix magnesium alloy to 700°C-750°C, and reducing the temperature to 560°C-600°C after the matrix alloy is completely melted to obtain a semi-solid molten magnesium alloy;

二、制备钛合金颗粒-镁合金混合熔体:将钛合金颗粒加热到100℃~200℃,预热20min~50min,然后将步骤一得到的半固态熔融镁合金在转速为600rpm~1000rpm的条件下进行搅拌,搅拌的同时将预热好的钛合金颗粒加入到半固态熔融镁合金中,继续在转速为1000rpm~1500rpm的条件下进行搅拌5min~10min,得到钛合金颗粒-镁合金混合熔体;其中,所述的钛合金颗粒与半固态熔融镁合金的体积比为1:(4~9);2. Preparation of titanium alloy particles-magnesium alloy mixed melt: heat the titanium alloy particles to 100°C-200°C, preheat for 20min-50min, and then melt the semi-solid molten magnesium alloy obtained in step 1 at a speed of 600rpm-1000rpm Stir under high temperature, while stirring, add the preheated titanium alloy particles into the semi-solid molten magnesium alloy, and continue stirring at a speed of 1000rpm to 1500rpm for 5min to 10min to obtain a titanium alloy particle-magnesium alloy mixed melt ; Wherein, the volume ratio of the titanium alloy particles to the semi-solid molten magnesium alloy is 1:(4~9);

三、制备钛合金颗粒增强镁基复合材料:将步骤二得到的钛合金颗粒-镁合金混合熔体在搅拌状态下加热至液态,在升温阶段采用转速最大的无涡流搅拌,转速为250rpm~300rpm,然后将液态混合熔体浇注到温度为400℃~450℃的模具中,并在100MPa~150MPa压力下凝固,即得到钛合金颗粒增强镁基复合材料。3. Preparation of titanium alloy particle-reinforced magnesium-based composite material: heat the titanium alloy particle-magnesium alloy mixed melt obtained in step 2 to a liquid state under stirring, and use the vortex-free stirring with the highest speed in the heating stage, and the speed is 250rpm~300rpm , and then pour the liquid mixed melt into a mold with a temperature of 400°C to 450°C and solidify under a pressure of 100MPa to 150MPa to obtain a titanium alloy particle reinforced magnesium matrix composite material.

本发明包含以下优点:The present invention comprises the following advantages:

本发明采用搅拌铸造方法制备了钛合金颗粒增强镁基复合材料,将镁合金先升温后降温形成半固态,然后将事先预热好的钛合金颗粒倒入到半固态熔体中同时进行半固态搅拌,搅拌预定时间后把混合熔体升温至液态,并将熔体浇注到模具中压铸成形。The invention adopts the stirring casting method to prepare the magnesium-based composite material reinforced with titanium alloy particles. The magnesium alloy is first heated up and then cooled to form a semi-solid state, and then the preheated titanium alloy particles are poured into the semi-solid melt and the semi-solid state is carried out at the same time. Stirring, after stirring for a predetermined time, the temperature of the mixed melt is raised to a liquid state, and the melt is poured into a mold for die-casting.

(1)本发明在制备过程中要对钛合金颗粒进行加热烘干,且预热温度为100℃~200℃,预热时间为20min~50min,这样既可以减少吸附在颗粒表面的气体量,提高颗粒与合金基体之间的润湿性,有利于颗粒的分散,又不至于使钛合金颗粒氧化严重,如果预热温度过高,就会使颗粒表面形成致密的TiO2层,这种陶瓷相就间隔了钛合金颗粒和基体之间的结合,会导致颗粒与基体之间界面结合较差;(1) In the preparation process of the present invention, titanium alloy particles should be heated and dried, and the preheating temperature is 100°C to 200°C, and the preheating time is 20min to 50min, so that the amount of gas adsorbed on the surface of the particles can be reduced, Improving the wettability between the particles and the alloy matrix is conducive to the dispersion of the particles without causing serious oxidation of the titanium alloy particles. If the preheating temperature is too high, a dense TiO2 layer will be formed on the surface of the particles. This ceramic The phase space between the titanium alloy particles and the matrix will lead to poor interfacial bonding between the particles and the matrix;

(2)本发明采用液态制备方法,充分发挥镁液在钛颗粒表面润湿性好的特点,因而钛合金颗粒与基体之间界面结合很好,且颗粒在合金熔体中易于分散,颗粒在基体中分布均匀,这样就可以使钛合金颗粒强度高和塑韧性好的特点得到充分发挥,从而提高镁基复合材料的综合性能,避免了其他方法如粉末冶金的颗粒与基体之间界面结合较差等问题;(2) The present invention adopts the liquid state preparation method, fully exerts the good wettability feature of magnesium liquid on the surface of titanium particles, thus the interface between titanium alloy particles and the substrate is well bonded, and the particles are easy to disperse in the alloy melt, and the particles are in The distribution in the matrix is uniform, so that the characteristics of high strength and good ductility of the titanium alloy particles can be fully utilized, thereby improving the comprehensive performance of the magnesium-based composite material, and avoiding the interface between the particles and the matrix in other methods such as powder metallurgy. Poor issues;

(3)本发明在半固态搅拌阶段搅拌时间较短,仅为5min~10min,这样就大大避免了因搅拌时间过长导致的氧化夹杂严重和气孔含量高的问题。这是因为钛与镁之间的润湿性特别好,搅拌较短时间就会使钛合金颗粒在基体中分散均匀;(3) The stirring time in the semi-solid stirring stage of the present invention is short, only 5min-10min, thus greatly avoiding the problems of serious oxidation inclusions and high pore content caused by too long stirring time. This is because the wettability between titanium and magnesium is particularly good, and the titanium alloy particles will be uniformly dispersed in the matrix after stirring for a short time;

(4)本发明可以方便地改变钛合金颗粒的体积分数和颗粒尺寸,制得各种体积分数和各种颗粒尺寸大小的钛合金颗粒增强的镁基复合材料;(4) The present invention can easily change the volume fraction and particle size of the titanium alloy particles, so that various volume fractions and various particle sizes of titanium alloy particle-reinforced magnesium-based composite materials can be obtained;

(5)本发明采用钛合金颗粒作为镁合金的增强体,与同体积分数同颗粒尺寸陶瓷颗粒(如SiC、TiC等)增强镁基复合材料相比,TC4p/AZ91镁基复合材料的强度和塑性都明显好于后者,可应用于航空航天、汽车、运动器械领域。(5) The present invention adopts titanium alloy particle as the reinforcing body of magnesium alloy, compares with the same volume fraction same particle size ceramic particle (as SiC, TiC etc.) reinforced magnesium-based composite material, the strength of TC4p/AZ91 magnesium-based composite material and The plasticity is obviously better than the latter, and it can be used in the fields of aerospace, automobiles, and sports equipment.

附图说明Description of drawings

图1为实施例1制备的TC4p/AZ91镁基复合材料的SEM图;Fig. 1 is the SEM figure of the TC4p/AZ91 magnesium-based composite material that embodiment 1 prepares;

图2为实施例2制备的TC4p/AZ91镁基复合材料的SEM图;Fig. 2 is the SEM figure of the TC4p/AZ91 magnesium-based composite material prepared in embodiment 2;

图3为实施例3制备的TC4p/AZ91镁基复合材料的SEM图;Fig. 3 is the SEM figure of the TC4p/AZ91 magnesium-based composite material prepared by embodiment 3;

图4为实施例4制备的TC4p/AZ91镁基复合材料的SEM图;Fig. 4 is the SEM figure of the TC4p/AZ91 magnesium-based composite material prepared by embodiment 4;

图5是AZ91镁合金和TC4p/AZ91镁基复合材料的拉伸曲线,曲线1为AZ91镁合金的拉伸曲线,曲线2是实施例1中制备的45μm10%TC4p/AZ91镁基复合材料的拉伸曲线,曲线3是实施例2中制备的45μm15%TC4p/AZ91镁基复合材料的拉伸曲线,曲线4是实施例3中制备的45μm20%TC4p/AZ91镁基复合材料的拉伸曲线,曲线5是实施例4中制备的25μm10%TC4p/AZ91镁基复合材料的拉伸曲线。Fig. 5 is the tensile curve of AZ91 magnesium alloy and TC4p/AZ91 magnesium-based composite material, and curve 1 is the tensile curve of AZ91 magnesium alloy, and curve 2 is the tensile curve of 45 μm10% TC4p/AZ91 magnesium-based composite material prepared in Example 1 Tensile curve, curve 3 is the tensile curve of the 45 μm 15% TC4p/AZ91 magnesium-based composite material prepared in Example 2, and curve 4 is the tensile curve of the 45 μm 20% TC4p/AZ91 magnesium-based composite material prepared in Example 3, the curve 5 is the tensile curve of the 25 μm 10% TC4p/AZ91 magnesium-based composite material prepared in Example 4.

具体实施方式Detailed ways

具体实施方式一:本实施方式的钛合金颗粒增强镁基复合材料的制备方法按以下步骤进行:Embodiment 1: The preparation method of the titanium alloy particle reinforced magnesium-based composite material of this embodiment is carried out according to the following steps:

一、制备半固态熔融镁合金:将基体镁合金升温至700℃~750℃,待基体合金完全熔化后将温度降至560℃~600℃,得到半固态熔融镁合金;1. Preparation of semi-solid molten magnesium alloy: raising the temperature of the matrix magnesium alloy to 700°C-750°C, and reducing the temperature to 560°C-600°C after the matrix alloy is completely melted to obtain a semi-solid molten magnesium alloy;

二、制备钛合金颗粒-镁合金混合熔体:将钛合金颗粒加热到100℃~200℃,预热20min~50min,然后将步骤一得到的半固态熔融镁合金在转速为600rpm~1000rpm的条件下进行搅拌,搅拌的同时将预热好的钛合金颗粒加入到半固态熔融镁合金中,继续在转速为1000rpm~1500rpm的条件下进行搅拌5min~10min,得到钛合金颗粒-镁合金混合熔体;其中,所述的钛合金颗粒与半固态熔融镁合金的体积比为1:(4~9);2. Preparation of titanium alloy particles-magnesium alloy mixed melt: heat the titanium alloy particles to 100°C-200°C, preheat for 20min-50min, and then melt the semi-solid molten magnesium alloy obtained in step 1 at a speed of 600rpm-1000rpm Stir under high temperature, while stirring, add the preheated titanium alloy particles into the semi-solid molten magnesium alloy, and continue stirring at a speed of 1000rpm to 1500rpm for 5min to 10min to obtain a titanium alloy particle-magnesium alloy mixed melt ; Wherein, the volume ratio of the titanium alloy particles to the semi-solid molten magnesium alloy is 1:(4~9);

三、制备钛合金颗粒增强镁基复合材料:将步骤二得到的钛合金颗粒-镁合金混合熔体在搅拌状态下加热至液态,然后将液态混合熔体浇注到温度为400℃~450℃的模具中,并在100MPa~150MPa压力下凝固,即得到钛合金颗粒增强镁基复合材料。3. Preparation of titanium alloy particle-reinforced magnesium-based composite material: the titanium alloy particle-magnesium alloy mixed melt obtained in step 2 is heated to a liquid state under stirring, and then the liquid mixed melt is poured to a temperature of 400°C to 450°C. and solidify under a pressure of 100 MPa to 150 MPa to obtain a titanium alloy particle reinforced magnesium matrix composite material.

具体实施方式二:本实施方式与具体实施方式一不同的是:步骤一中将镁合金基体升温至710℃~740℃,然后将温度降至570℃~600℃,得到半固态熔融镁合金。其它与具体实施方式一相同。Embodiment 2: This embodiment differs from Embodiment 1 in that in step 1, the magnesium alloy substrate is heated to 710°C-740°C, and then the temperature is lowered to 570°C-600°C to obtain a semi-solid molten magnesium alloy. Others are the same as in the first embodiment.

具体实施方式三:本实施方式与具体实施方式一不同的是:步骤一中将镁合金基体升温至720℃~730℃,然后将温度降至580℃~600℃,得到半固态熔融镁合金。其它与具体实施方式一相同。Embodiment 3: This embodiment differs from Embodiment 1 in that in step 1, the magnesium alloy substrate is heated to 720°C-730°C, and then the temperature is lowered to 580°C-600°C to obtain a semi-solid molten magnesium alloy. Others are the same as in the first embodiment.

具体实施方式四:本实施方式与具体实施方式一不同的是:步骤一中将镁合金基体升温至720℃~730℃,然后将温度降至590℃~600℃,得到半固态熔融镁合金。其它与具体实施方式一相同。Embodiment 4: This embodiment differs from Embodiment 1 in that in step 1, the magnesium alloy substrate is heated to 720°C-730°C, and then the temperature is lowered to 590°C-600°C to obtain a semi-solid molten magnesium alloy. Others are the same as in the first embodiment.

具体实施方式五:本实施方式与具体实施方式一不同的是:步骤二中钛合金的预热温度为120℃~180℃,预热时间为30min~50min,然后将步骤一得到的半固态熔融镁合金在转速为600rpm~1000rpm的条件下进行搅拌,同时将预热颗粒倒入到镁合金半固态熔体中,继续在1000rpm~1500rpm的条件下进行搅拌,搅拌时间为6min~10min,并且所述的钛合金颗粒与半固态熔融镁合金的体积比为1:(5~8)。其它与具体实施方式一相同。Embodiment 5: This embodiment differs from Embodiment 1 in that the preheating temperature of the titanium alloy in step 2 is 120°C to 180°C, and the preheating time is 30min to 50min, and then the semi-solid obtained in step 1 is melted Stir the magnesium alloy at a rotational speed of 600rpm-1000rpm, pour the preheated particles into the magnesium alloy semi-solid melt, and continue stirring at 1000rpm-1500rpm for 6min-10min, and the The volume ratio of the titanium alloy particles to the semi-solid molten magnesium alloy is 1:(5-8). Others are the same as in the first embodiment.

具体实施方式六:本实施方式与具体实施方式一不同的是:步骤二中钛合金的预热温度为140℃~160℃,预热时间为40min~50min,然后将步骤一得到的半固态熔融镁合金在转速为600rpm~1000rpm的条件下进行搅拌,同时将预热颗粒倒入到镁合金半固态熔体中,继续在1000rpm~1500rpm的条件下进行搅拌,搅拌时间为8min~10min,并且所述的钛合金颗粒与半固态熔融镁合金的体积比为1:(6~7)。其它与具体实施方式一相同。Embodiment 6: This embodiment is different from Embodiment 1 in that the preheating temperature of the titanium alloy in step 2 is 140°C to 160°C, and the preheating time is 40min to 50min, and then the semi-solid obtained in step 1 is melted Stir the magnesium alloy at a rotational speed of 600rpm-1000rpm, pour the preheated particles into the magnesium alloy semi-solid melt, and continue stirring at 1000rpm-1500rpm for 8min-10min, and the The volume ratio of the titanium alloy particles to the semi-solid molten magnesium alloy is 1:(6-7). Others are the same as in the first embodiment.

具体实施方式七:本实施方式与具体实施方式一不同的是:步骤二中钛合金的预热温度为150℃,预热时间为45min,然后将步骤一得到的半固态熔融镁合金在转速为600rpm~1000rpm的条件下进行搅拌,同时将预热颗粒倒入到镁合金半固态熔体中,继续在1000rpm~1500rpm的条件下进行搅拌,搅拌时间为9min,并且所述的钛合金颗粒与半固态熔融镁合金的体积比为1:(6~7)。其它与具体实施方式一相同。Specific embodiment seven: the difference between this embodiment and specific embodiment one is: the preheating temperature of the titanium alloy in step two is 150 DEG C, and the preheating time is 45min, and then the semi-solid molten magnesium alloy obtained in step one is rotated at a speed of Stir under the condition of 600rpm~1000rpm, pour the preheated particles into the magnesium alloy semi-solid melt at the same time, continue to stir under the condition of 1000rpm~1500rpm, the stirring time is 9min, and the titanium alloy particles and semi-solid The volume ratio of solid molten magnesium alloy is 1:(6~7). Others are the same as in the first embodiment.

具体实施方式八:本实施方式与具体实施方式一不同的是:步骤三中将步骤二得到的合金熔体加热至液态,然后将液态的合金熔体浇注到温度为420℃~450℃的模具中并在120MPa~150MPa压力下凝固,得到钛合金颗粒增强镁基复合材料。其它与具体实施方式一相同。Embodiment 8: The difference between this embodiment and Embodiment 1 is that in step 3, the alloy melt obtained in step 2 is heated to a liquid state, and then the liquid alloy melt is poured into a mold with a temperature of 420°C to 450°C and solidify under a pressure of 120MPa to 150MPa to obtain a titanium alloy particle reinforced magnesium matrix composite material. Others are the same as in the first embodiment.

具体实施方式九:本实施方式与具体实施方式一不同的是:步骤三中将步骤二得到的合金熔体加热至液态,然后将液态的合金熔体浇注到温度为430℃~450℃的模具中并在130MPa~150MPa压力下凝固,得到钛合金颗粒增强镁基复合材料。其它与具体实施方式一相同。Embodiment 9: The difference between this embodiment and Embodiment 1 is that in Step 3, the alloy melt obtained in Step 2 is heated to a liquid state, and then the liquid alloy melt is poured into a mold with a temperature of 430°C to 450°C and solidify under a pressure of 130MPa-150MPa to obtain a titanium alloy particle reinforced magnesium matrix composite material. Others are the same as in the first embodiment.

具体实施方式十:本实施方式与具体实施方式一不同的是:步骤一中所述的基体镁合金为AZ91镁合金。其它与具体实施方式一相同。Embodiment 10: This embodiment is different from Embodiment 1 in that the matrix magnesium alloy described in step 1 is AZ91 magnesium alloy. Others are the same as in the first embodiment.

具体实施方式十一:本实施方式与具体实施方式一不同的是:步骤三中钛合金颗粒-镁合金混合熔体在搅拌状态下加热至液态中所述的搅拌是采用转速最大的无涡流搅拌,转速为250rpm~300rpm。其它与具体实施方式一相同。Embodiment 11: The difference between this embodiment and Embodiment 1 is that in Step 3, the titanium alloy particle-magnesium alloy mixed melt is heated to a liquid state under stirring. , the speed is 250rpm ~ 300rpm. Others are the same as in the first embodiment.

下面结合本发明的内容提供以下实施例:Provide following embodiment below in conjunction with content of the present invention:

实施例1:Example 1:

本实施例的钛合金颗粒增强镁基复合材料的制备方法按以下步骤进行:The preparation method of the titanium alloy particle reinforced magnesium-based composite material of this embodiment is carried out according to the following steps:

(1)制备半固态熔融镁合金:将基体AZ91镁合金升温至700℃~750℃,待基体合金完全熔化后将温度降至560℃~600℃,得到半固态熔融镁合金;(1) Preparation of semi-solid molten magnesium alloy: heating the base AZ91 magnesium alloy to 700°C-750°C, and reducing the temperature to 560°C-600°C after the base alloy is completely melted to obtain a semi-solid molten magnesium alloy;

(2)制备钛合金颗粒-镁合金混合熔体:将平均粒径为45μm的TC4钛合金颗粒加热到100℃~200℃,预热20min~50min,然后将步骤(1)得到的半固态熔融镁合金进行搅拌,转速为600rpm~1000rpm,与此同时将预热好的钛合金颗粒加入到半固态熔融镁合金中,继续在转速为1000rpm~1500rpm的条件下进行搅拌5min,得到钛合金颗粒-镁合金混合熔体,步骤(2)所述的钛合金颗粒与半固态熔融镁合金的体积比为1:9;(2) Preparation of titanium alloy particle-magnesium alloy mixed melt: heat TC4 titanium alloy particles with an average particle size of 45 μm to 100°C-200°C, preheat for 20min-50min, and then melt the semi-solid obtained in step (1) The magnesium alloy is stirred at a speed of 600rpm to 1000rpm. At the same time, the preheated titanium alloy particles are added to the semi-solid molten magnesium alloy, and the stirring is continued at a speed of 1000rpm to 1500rpm for 5 minutes to obtain titanium alloy particles- Magnesium alloy mixed melt, the volume ratio of titanium alloy particles described in step (2) and semi-solid molten magnesium alloy is 1:9;

(3)制备钛合金颗粒增强镁基复合材料:将步骤(2)得到的钛合金颗粒-镁合金混合熔体升温至液态,在升温阶段采用转速最大的无涡流搅拌,转速为250rpm~300rpm,然后将液态混合熔体浇注到温度为400℃~450℃的模具中,并在100MPa~150MPa压力下凝固,得到钛合金颗粒增强镁基复合材料。(3) Preparation of titanium alloy particle-reinforced magnesium-based composite material: the titanium alloy particle-magnesium alloy mixed melt obtained in step (2) is heated to a liquid state, and the vortex-free stirring with the largest rotating speed is used in the heating stage, and the rotating speed is 250rpm~300rpm, Then pour the liquid mixed melt into a mold with a temperature of 400°C to 450°C and solidify under a pressure of 100MPa to 150MPa to obtain a titanium alloy particle reinforced magnesium matrix composite material.

实施例2:Example 2:

本实施例的钛合金颗粒增强镁基复合材料的制备方法按以下步骤进行:The preparation method of the titanium alloy particle reinforced magnesium-based composite material of this embodiment is carried out according to the following steps:

(1)制备半固态熔融镁合金:将基体AZ91镁合金升温至700℃~750℃,待基体合金完全熔化后将温度降至560℃~600℃,得到半固态熔融镁合金;(1) Preparation of semi-solid molten magnesium alloy: heating the base AZ91 magnesium alloy to 700°C-750°C, and reducing the temperature to 560°C-600°C after the base alloy is completely melted to obtain a semi-solid molten magnesium alloy;

(2)制备钛合金颗粒-镁合金混合熔体:将平均粒径为45μm的TC4钛合金颗粒加热到100℃~200℃,预热20min~50min,然后将步骤(1)得到的半固态熔融镁合金进行搅拌,转速为600rpm~1000rpm,与此同时将预热好的钛合金颗粒加入到半固态熔融镁合金中,继续在转速为1000rpm~1500rpm的条件下进行搅拌7min,得到钛合金颗粒-镁合金混合熔体,步骤(2)所述的钛合金颗粒与半固态熔融镁合金的体积比为3:17;(2) Preparation of titanium alloy particle-magnesium alloy mixed melt: heat TC4 titanium alloy particles with an average particle size of 45 μm to 100°C-200°C, preheat for 20min-50min, and then melt the semi-solid obtained in step (1) The magnesium alloy is stirred at a speed of 600rpm to 1000rpm. At the same time, the preheated titanium alloy particles are added to the semi-solid molten magnesium alloy, and the stirring is continued at a speed of 1000rpm to 1500rpm for 7 minutes to obtain titanium alloy particles- Magnesium alloy mixed melt, the volume ratio of titanium alloy particles described in step (2) and semi-solid molten magnesium alloy is 3:17;

(3)制备钛合金颗粒增强镁基复合材料:将步骤(2)得到的钛合金颗粒-镁合金混合熔体升温至液态,在升温阶段采用转速最大的无涡流搅拌,转速为250rpm~300rpm,然后将液态混合熔体浇注到温度为400℃~450℃的模具中,并在100MPa~150MPa压力下凝固,得到钛合金颗粒增强镁基复合材料。(3) Preparation of titanium alloy particle-reinforced magnesium-based composite material: the titanium alloy particle-magnesium alloy mixed melt obtained in step (2) is heated to a liquid state, and the vortex-free stirring with the largest rotating speed is used in the heating stage, and the rotating speed is 250rpm~300rpm, Then pour the liquid mixed melt into a mold with a temperature of 400°C to 450°C and solidify under a pressure of 100MPa to 150MPa to obtain a titanium alloy particle reinforced magnesium matrix composite material.

实施例3:Example 3:

本实施例的钛合金颗粒增强镁基复合材料的制备方法按以下步骤进行:The preparation method of the titanium alloy particle reinforced magnesium-based composite material of this embodiment is carried out according to the following steps:

(1)制备半固态熔融镁合金:将基体AZ91镁合金升温至700℃~750℃,待基体合金完全熔化后将温度降至560℃~600℃,得到半固态熔融镁合金;(1) Preparation of semi-solid molten magnesium alloy: heating the base AZ91 magnesium alloy to 700°C-750°C, and reducing the temperature to 560°C-600°C after the base alloy is completely melted to obtain a semi-solid molten magnesium alloy;

(2)制备钛合金颗粒-镁合金混合熔体:将平均粒径为45μm的TC4钛合金颗粒加热到100℃~200℃,预热20min~50min,然后将步骤(1)得到的半固态熔融镁合金进行搅拌,转速为600rpm~1000rpm,与此同时将预热好的钛合金颗粒加入到半固态熔融镁合金中,继续在转速为1000rpm~1500rpm的条件下进行搅拌10min,得到钛合金颗粒-镁合金混合熔体,步骤(2)所述的钛合金颗粒与半固态熔融镁合金的体积比为1:4;(2) Preparation of titanium alloy particle-magnesium alloy mixed melt: heat TC4 titanium alloy particles with an average particle size of 45 μm to 100°C-200°C, preheat for 20min-50min, and then melt the semi-solid obtained in step (1) The magnesium alloy is stirred at a speed of 600rpm to 1000rpm. At the same time, the preheated titanium alloy particles are added to the semi-solid molten magnesium alloy, and the stirring is continued at a speed of 1000rpm to 1500rpm for 10 minutes to obtain titanium alloy particles- Magnesium alloy mixed melt, the volume ratio of titanium alloy particles described in step (2) and semi-solid molten magnesium alloy is 1:4;

(3)制备钛合金颗粒增强镁基复合材料:将步骤(2)得到的钛合金颗粒-镁合金混合熔体升温至液态,在升温阶段采用转速最大的无涡流搅拌,转速为250rpm~300rpm,然后将液态混合熔体浇注到温度为400℃~450℃的模具中,并在100MPa~150MPa压力下凝固,得到钛合金颗粒增强镁基复合材料。(3) Preparation of titanium alloy particle-reinforced magnesium-based composite material: the titanium alloy particle-magnesium alloy mixed melt obtained in step (2) is heated to a liquid state, and the vortex-free stirring with the largest rotating speed is used in the heating stage, and the rotating speed is 250rpm~300rpm, Then pour the liquid mixed melt into a mold with a temperature of 400°C to 450°C and solidify under a pressure of 100MPa to 150MPa to obtain a titanium alloy particle reinforced magnesium matrix composite material.

实施例4:Example 4:

本实施例的钛合金颗粒增强镁基复合材料的制备方法按以下步骤进行:The preparation method of the titanium alloy particle reinforced magnesium-based composite material of this embodiment is carried out according to the following steps:

(1)制备半固态熔融镁合金:将基体AZ91镁合金升温至700℃~750℃,待基体合金完全熔化后将温度降至560℃~600℃,得到半固态熔融镁合金;(1) Preparation of semi-solid molten magnesium alloy: heating the base AZ91 magnesium alloy to 700°C-750°C, and reducing the temperature to 560°C-600°C after the base alloy is completely melted to obtain a semi-solid molten magnesium alloy;

(2)制备钛合金颗粒-镁合金混合熔体:将平均粒径为25μm的TC4钛合金颗粒加热到100℃~200℃,预热20min~50min,然后将步骤(1)得到的半固态熔融镁合金进行搅拌,转速为600rpm~1000rpm,与此同时将预热好的钛合金颗粒加入到半固态熔融镁合金中,继续在转速为1000rpm~1500rpm的条件下进行搅拌7min,得到钛合金颗粒-镁合金混合熔体,步骤(2)所述的钛合金颗粒与半固态熔融镁合金的体积比为1:9;(2) Preparation of titanium alloy particles-magnesium alloy mixed melt: heat TC4 titanium alloy particles with an average particle size of 25 μm to 100°C-200°C, preheat for 20min-50min, and then melt the semi-solid obtained in step (1) The magnesium alloy is stirred at a speed of 600rpm to 1000rpm. At the same time, the preheated titanium alloy particles are added to the semi-solid molten magnesium alloy, and the stirring is continued at a speed of 1000rpm to 1500rpm for 7 minutes to obtain titanium alloy particles- Magnesium alloy mixed melt, the volume ratio of titanium alloy particles described in step (2) and semi-solid molten magnesium alloy is 1:9;

(3)制备钛合金颗粒增强镁基复合材料:将步骤(2)得到的钛合金颗粒-镁合金混合熔体升温至液态,在升温阶段采用转速最大的无涡流搅拌,转速为250rpm~300rpm,然后将液态混合熔体浇注到温度为400℃~450℃的模具中,并在100MPa~150MPa压力下凝固,得到钛合金颗粒增强镁基复合材料。所制备材料的性能见表1所示。(3) Preparation of titanium alloy particle-reinforced magnesium-based composite material: the titanium alloy particle-magnesium alloy mixed melt obtained in step (2) is heated to a liquid state, and the vortex-free stirring with the largest rotating speed is used in the heating stage, and the rotating speed is 250rpm~300rpm, Then pour the liquid mixed melt into a mold with a temperature of 400°C to 450°C and solidify under a pressure of 100MPa to 150MPa to obtain a titanium alloy particle reinforced magnesium matrix composite material. The properties of the prepared materials are shown in Table 1.

表1  AZ91镁合金和本发明制备的TC4p/AZ91镁基复合材料的力学性能Table 1 AZ91 magnesium alloy and the mechanical properties of the TC4p/AZ91 magnesium-based composite material prepared by the present invention

图1为实施例1制备的TC4p/AZ91镁基复合材料的SEM图,图2为实施例2制备的TC4p/AZ91镁基复合材料的SEM图,图3为实施例3制备的TC4p/AZ91镁基复合材料的SEM图,图4为实施例4制备的TC4p/AZ91镁基复合材料的SEM图,可以看出:TC4钛合金颗粒在基体中分布都非常均匀,没有明显的团聚现象,实现了TC4钛合金颗粒的均匀分散。Fig. 1 is the SEM picture of the TC4p/AZ91 magnesium-based composite material prepared in Example 1, Fig. 2 is the SEM picture of the TC4p/AZ91 magnesium-based composite material prepared in Example 2, and Fig. 3 is the TC4p/AZ91 magnesium-based composite material prepared in Example 3 The SEM image of the matrix composite material, Figure 4 is the SEM image of the TC4p/AZ91 magnesium-based composite material prepared in Example 4, it can be seen that: the TC4 titanium alloy particles are very uniformly distributed in the matrix, and there is no obvious agglomeration phenomenon. Uniform dispersion of TC4 titanium alloy particles.

图5是AZ91镁合金和TC4p/AZ91镁基复合材料的拉伸曲线,曲线1为AZ91镁合金的拉伸曲线,曲线2是实施例1中制备的45μm10%TC4p/AZ91镁基复合材料的拉伸曲线,曲线3是实施例2中制备的45μm15%TC4p/AZ91镁基复合材料的拉伸曲线,曲线4是实施例3中制备的45μm20%TC4p/AZ91镁基复合材料的拉伸曲线,曲线5是实施例4中制备的25μm10%TC4p/AZ91镁基复合材料的拉伸曲线,可以看出:与AZ91镁合金相比,TC4p/AZ91镁基复合材料的强度明显提高,并且随着颗粒体积分数的升高或颗粒尺寸的减小,TC4p/AZ91镁基复合材料的强度也随之显著提高。Fig. 5 is the tensile curve of AZ91 magnesium alloy and TC4p/AZ91 magnesium-based composite material, and curve 1 is the tensile curve of AZ91 magnesium alloy, and curve 2 is the tensile curve of 45 μm10% TC4p/AZ91 magnesium-based composite material prepared in Example 1 Tensile curve, curve 3 is the tensile curve of the 45 μm 15% TC4p/AZ91 magnesium-based composite material prepared in Example 2, and curve 4 is the tensile curve of the 45 μm 20% TC4p/AZ91 magnesium-based composite material prepared in Example 3, the curve 5 is the tensile curve of the 25 μm 10% TC4p/AZ91 magnesium-based composite material prepared in Example 4. It can be seen that: compared with the AZ91 magnesium alloy, the strength of the TC4p/AZ91 magnesium-based composite material is significantly improved, and the particle volume increases The strength of TC4p/AZ91 magnesium matrix composites also increases significantly with the increase of fraction or the decrease of particle size.

Claims (10)

1. titanium alloy particle strengthens a preparation method for magnesium base composite material, it is characterized in that this preparation method carries out according to the following steps:
One, semi-solid state molten magnesium alloy is prepared: matrix magnesium alloy is warming up to 700 DEG C ~ 750 DEG C, after matrix alloy melts completely, cools the temperature to 560 DEG C ~ 600 DEG C, obtain semi-solid state molten magnesium alloy;
Two, titanium alloy particle-magnesium alloy blend melt is prepared: titanium alloy particle is heated to 100 DEG C ~ 200 DEG C, preheating 20min ~ 50min, then semi-solid state molten magnesium alloy step one obtained is stir under the condition of 600rpm ~ 1000rpm at rotating speed, while stirring, preheated titanium alloy particle is joined in semi-solid state molten magnesium alloy, continue to carry out stirring 5min ~ 10min under rotating speed is the condition of 1000rpm ~ 1500rpm, obtain titanium alloy particle-magnesium alloy blend melt; Wherein, the volume ratio of described titanium alloy particle and semi-solid state molten magnesium alloy is 1:(4 ~ 9);
Three, prepare titanium alloy particle and strengthen magnesium base composite material: titanium alloy particle step 2 obtained-magnesium alloy blend melt is heated to liquid state under whipped state, the temperature rise period adopt rotating speed maximum without vortex stirring, rotating speed is 250rpm ~ 300rpm, then liquid blend melt being poured into temperature is in the mould of 400 DEG C ~ 450 DEG C, and at 100MPa ~ 150MPa Under Pressure Solidification, namely obtain titanium alloy particle and strengthen magnesium base composite material.
2. a kind of titanium alloy particle according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that magnesium alloy substrate being warming up to 710 DEG C ~ 740 DEG C in step one, then cool the temperature to 570 DEG C ~ 600 DEG C, obtain semi-solid state molten magnesium alloy.
3. a kind of titanium alloy particle according to claim 2 strengthens the preparation method of magnesium base composite material, it is characterized in that magnesium alloy substrate being warming up to 720 DEG C ~ 730 DEG C in step one, then cool the temperature to 580 DEG C ~ 600 DEG C, obtain semi-solid state molten magnesium alloy.
4. a kind of titanium alloy particle according to claim 3 strengthens the preparation method of magnesium base composite material, it is characterized in that magnesium alloy substrate being warming up to 720 DEG C ~ 730 DEG C in step one, then cool the temperature to 590 DEG C ~ 600 DEG C, obtain semi-solid state molten magnesium alloy.
5. a kind of titanium alloy particle according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that the preheating temperature of titanium alloy in step 2 is 120 DEG C ~ 180 DEG C, warm up time is 30min ~ 50min, then semi-solid state molten magnesium alloy step one obtained is stir under the condition of 600rpm ~ 1000rpm at rotating speed, preheating particulate is poured in magnesium alloy semi solid state melt simultaneously, continue to stir under the condition of 1000rpm ~ 1500rpm, churning time is 6min ~ 10min, and the volume ratio of described titanium alloy particle and semi-solid state molten magnesium alloy is 1:(5 ~ 8).
6. a kind of titanium alloy particle according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that the preheating temperature of titanium alloy in step 2 is 140 DEG C ~ 160 DEG C, warm up time is 40min ~ 50min, then semi-solid state molten magnesium alloy step one obtained is stir under the condition of 600rpm ~ 1000rpm at rotating speed, preheating particulate is poured in magnesium alloy semi solid state melt simultaneously, continue to stir under the condition of 1000rpm ~ 1500rpm, churning time is 8min ~ 10min, and the volume ratio of described titanium alloy particle and semi-solid state molten magnesium alloy is 1:(6 ~ 7).
7. a kind of titanium alloy particle according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that the preheating temperature of titanium alloy in step 2 is 150 DEG C, warm up time is 45min, then semi-solid state molten magnesium alloy step one obtained is stir under the condition of 600rpm ~ 1000rpm at rotating speed, preheating particulate is poured in magnesium alloy semi solid state melt simultaneously, continue to stir under the condition of 1000rpm ~ 1500rpm, churning time is 9min, and the volume ratio of described titanium alloy particle and semi-solid state molten magnesium alloy is 1:(6 ~ 7).
8. a kind of titanium alloy particle according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that, in step 3, the alloy melt that step 2 obtains is heated to liquid state, then the alloy melt of liquid state being poured into temperature is in the mould of 420 DEG C ~ 450 DEG C and at 120MPa ~ 150MPa Under Pressure Solidification, obtains titanium alloy particle and strengthens magnesium base composite material.
9. a kind of titanium alloy particle according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that, in step 3, the alloy melt that step 2 obtains is heated to liquid state, then the alloy melt of liquid state being poured into temperature is in the mould of 430 DEG C ~ 450 DEG C and at 130MPa ~ 150MPa Under Pressure Solidification, obtains titanium alloy particle and strengthens magnesium base composite material.
10. a kind of titanium alloy particle according to claim 1 strengthens the preparation method of magnesium base composite material, it is characterized in that the matrix magnesium alloy described in step one is AZ91 magnesium alloy.
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CN107513651A (en) * 2017-09-08 2017-12-26 燕山大学 A kind of preparation method of titanium particle reinforced magnesium base composite material
CN107513651B (en) * 2017-09-08 2019-07-26 燕山大学 A kind of preparation method of titanium particle reinforced magnesium matrix composite material
CN109022859A (en) * 2018-09-17 2018-12-18 太原理工大学 A kind of preparation method of nano-titanium particulate reinforcement magnesium-based composite material
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CN113493876B (en) * 2021-07-07 2022-07-01 重庆大学 A kind of method of iron-based amorphous modified magnesium alloy surface
CN113493876A (en) * 2021-07-07 2021-10-12 重庆大学 Method for modifying surface of magnesium alloy through iron-based amorphous modification
CN114438385A (en) * 2022-01-28 2022-05-06 重庆大学 A kind of preparation method of metal titanium particle reinforced magnesium matrix composite material
CN114959391A (en) * 2022-05-30 2022-08-30 广东省科学院新材料研究所 Titanium particle reinforced magnesium-based composite material and preparation method thereof
CN114959391B (en) * 2022-05-30 2023-01-06 广东省科学院新材料研究所 A kind of titanium particle reinforced magnesium-based composite material and preparation method thereof
CN115074560A (en) * 2022-06-30 2022-09-20 广东省科学院新材料研究所 Titanium particle reinforced magnesium-based composite material and preparation method thereof
CN115074560B (en) * 2022-06-30 2023-03-14 广东省科学院新材料研究所 Titanium particle reinforced magnesium matrix composite material and preparation method thereof
CN115852181A (en) * 2022-11-28 2023-03-28 重庆大学 Preparation method of micron-sized titanium particle reinforced magnesium-based composite material
CN115852181B (en) * 2022-11-28 2023-09-01 重庆大学 A kind of preparation method of micron-scale titanium particle reinforced magnesium-based composite material
CN119410923A (en) * 2024-10-10 2025-02-11 广东省科学院新材料研究所 A magnesium-based composite material and its preparation method and application

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