CN110643851A - A kind of TiAl matrix composite material and its thermomechanical treatment method - Google Patents

A kind of TiAl matrix composite material and its thermomechanical treatment method Download PDF

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CN110643851A
CN110643851A CN201910982445.7A CN201910982445A CN110643851A CN 110643851 A CN110643851 A CN 110643851A CN 201910982445 A CN201910982445 A CN 201910982445A CN 110643851 A CN110643851 A CN 110643851A
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李臻熙
高帆
齐立春
刘宏武
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AECC Beijing Institute of Aeronautical Materials
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    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • C22C32/0073Non-ferrous alloys containing at least 5% by weight but less than 50% by weight of oxides, carbides, borides, nitrides, silicides or other metal compounds, e.g. oxynitrides, sulfides, whether added as such or formed in situ with carbides, nitrides, borides or silicides as the main non-metallic constituents only borides
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    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
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Abstract

本发明涉及一种以原位自生成的TiB2晶须增强的TiAl基复合材料及其热机械处理方法。根据B元素添加控制量计算公式,在TiAl合金中添加适量的B元素,使得在TiAl合金中形成以L→β+TiB2和L+β→α+TiB2共晶反应原位自生成细长的次生TiB2晶须,同时避免粗大的颗粒状初生TiB2相产生,从而可以通过铸锭冶金方法制备一种TiB2晶须增强的TiAl基复合材料。而后,TiB2/TiAl复合材料经过包套热挤压或者包套锻造可制备成细晶棒材或者细晶饼坯,细长TiB2晶须被破碎成短晶须,再经过特殊的热处理工艺的处理,可以获得细晶网篮状组织或者细晶全片层组织。这种TiB2/TiAl复合材料从室温一直到850℃高温均具有很高的强度,同时还具有优异的室温塑性,因此在航空航天领域具有良好的应用前景。

Figure 201910982445

The invention relates to a TiAl-based composite material reinforced with in-situ self-generated TiB2 whiskers and a thermomechanical treatment method thereof. According to the calculation formula of B element addition control amount, an appropriate amount of B element is added to the TiAl alloy, so that the in-situ self-generated slender secondary eutectic reaction of L→β+TiB2 and L+β→α+TiB2 is formed in the TiAl alloy. While avoiding the generation of coarse granular primary TiB2 phase, a TiB2 whisker reinforced TiAl-based composite material can be prepared by ingot-casting metallurgical method. Then, the TiB2/TiAl composite material can be prepared into fine-grained rods or fine-grained cake blanks by wrapping hot extrusion or wrapping forging, and the slender TiB2 whiskers are broken into short whiskers, which are then treated by a special heat treatment process. , a fine-grained basket-like structure or a fine-grained full-sheet structure can be obtained. This TiB2/TiAl composite has high strength from room temperature to high temperature of 850 °C, and also has excellent room temperature plasticity, so it has a good application prospect in the aerospace field.

Figure 201910982445

Description

一种TiAl基复合材料及其热机械处理方法A kind of TiAl matrix composite material and its thermomechanical treatment method

技术领域technical field

本发明属于复合材料制备领域,涉及一种TiAl基复合材料及其热机械处理方法,具体涉及一种原位自生成TiB2晶须增强TiAl基复合材料及其热加工和热处理方法。The invention belongs to the field of composite material preparation, relates to a TiAl matrix composite material and a thermomechanical treatment method thereof, in particular to an in-situ self-generated TiB2 whisker reinforced TiAl matrix composite material and a thermal processing and heat treatment method thereof.

背景技术Background technique

γ-TiAl基金属间化合物合金具有低密度、高比强度、高比模量、高蠕变抗力、抗氧化、抗燃烧等优异的性能,因此成为新一代高温结构材料而倍受关注,目前已经成为新一代高推重比航空发动机的关键材料。γ-TiAl-based intermetallic compound alloys have excellent properties such as low density, high specific strength, high specific modulus, high creep resistance, oxidation resistance, and combustion resistance, so they have attracted much attention as a new generation of high-temperature structural materials. Become a key material for a new generation of high thrust-to-weight ratio aero-engines.

通过在TiAl合金中添加颗粒状、纤维状增强体制备成TiAl基复合材料,可提高TiAl合金的高温强度和高温持久性能。但是由于TiAl合金室温塑性只有1~2%,当在TiAl合金中添加增强体会导致室温塑性进一步降低,因此往往难以制备出大尺寸的TiAl基复合材料。TiAl基复合材料的增强体和基体在制备过程中经常会发生强烈的界面反应,导致复合材料的性能显著降低。例如,采用粉末冶金方法制备SiC纤维增强TiAl基复合材料,因为SiC纤维和TiAl合金线膨胀系数相差太大,因而冷却过程中产生的热应力导致沿SiC纤维的径向产生裂纹。采用粉末冶金方法制备Al2O3纤维增强TiAl复合材料,发现Al2O3纤维与TiAl基体的界面反应异常剧烈。粉末冶金的TiAl复合材料热加工性能非常差,在热变形过程中增强体附近会产生强烈的应力应变集中,从而形成裂纹。The high temperature strength and high temperature durability of TiAl alloy can be improved by adding granular and fibrous reinforcement to TiAl alloy to prepare TiAl matrix composite material. However, since the room temperature plasticity of TiAl alloy is only 1-2%, when adding reinforcement to TiAl alloy, the room temperature plasticity will be further reduced, so it is often difficult to prepare large-sized TiAl matrix composites. The reinforcement and matrix of TiAl-based composites often undergo strong interfacial reactions during the preparation process, resulting in a significant decrease in the performance of the composites. For example, the powder metallurgy method is used to prepare SiC fiber reinforced TiAl matrix composites. Because the linear expansion coefficients of SiC fibers and TiAl alloys are too different, the thermal stress generated during the cooling process leads to cracks along the radial direction of the SiC fibers. Al 2 O 3 fiber reinforced TiAl composites were prepared by powder metallurgy method, and it was found that the interface reaction between Al 2 O 3 fibers and TiAl matrix was extremely violent. The thermal processing performance of powder metallurgy TiAl composites is very poor. During the hot deformation process, a strong concentration of stress and strain occurs near the reinforcement, resulting in the formation of cracks.

发明内容SUMMARY OF THE INVENTION

本发明的目的是:提供一种TiAl基复合材料及其热机械处理方法,以解决目前TiAl基复合材料基体与增强体发生界面反应或界面附近应力集中产生较大脆性,难以制备出高强塑性TiAl基复合材料的技术问题。The purpose of the present invention is to provide a TiAl-based composite material and a thermomechanical treatment method thereof, so as to solve the problem that the interface reaction between the matrix and the reinforcement of the current TiAl-based composite material or the stress concentration near the interface produces greater brittleness, and it is difficult to prepare high-strength plastic TiAl Technical issues of matrix composites.

为解决此技术问题,本发明的技术方案是:In order to solve this technical problem, the technical scheme of the present invention is:

一方面,本发明提供一种TiAl基复合材料,所述的TiAl基复合材料按原子百分含量含有:0.5%~1.5%B、42%~45.5%Al、1%~2%Cr、3%~6%Nb、0.1%~0.5%Ta、0~0.2%Si、0%~2%C,余量为Ti和不可避免的杂质,其中氧含量≤0.2wt%、氮含量≤0.03wt%、氢含量≤0.02wt%;In one aspect, the present invention provides a TiAl-based composite material, the TiAl-based composite material contains by atomic percentage: 0.5%-1.5% B, 42%-45.5% Al, 1%-2% Cr, 3% ~6%Nb, 0.1%~0.5%Ta, 0~0.2%Si, 0%~2%C, the balance is Ti and inevitable impurities, of which oxygen content≤0.2wt%, nitrogen content≤0.03wt%, Hydrogen content≤0.02wt%;

所述的TiAl基复合材料的弹性模量E≥150GPa;The elastic modulus of the TiAl-based composite material is E≥150GPa;

所述的TiAl基复合材料的增强体为弥散分布的TiB2短晶须;晶须长度≤30μm。The reinforcing body of the TiAl-based composite material is a dispersion-distributed TiB 2 short whisker; the whisker length is less than or equal to 30 μm.

优选地,本发明提供一种TiAl基复合材料,所述的TiAl基复合材料按原子百分含量含有:45.5%Al、0.5%B、1.5%Cr、4%Nb、0.2%Ta、0.2%Si,余量为Ti和不可避免的杂质。Preferably, the present invention provides a TiAl-based composite material, the TiAl-based composite material contains by atomic percentage: 45.5% Al, 0.5% B, 1.5% Cr, 4% Nb, 0.2% Ta, 0.2% Si , the remainder is Ti and inevitable impurities.

优选地,本发明提供另一种TiAl基复合材料,所述的TiAl基复合材料按原子百分含量含有:44%Al、0.8%B、1%Cr、4%Nb、0.2%Ta,余量为Ti和不可避免的杂质。Preferably, the present invention provides another TiAl-based composite material, the TiAl-based composite material contains by atomic percentage: 44% Al, 0.8% B, 1% Cr, 4% Nb, 0.2% Ta, the remainder for Ti and inevitable impurities.

优选地,本发明提供第三种TiAl基复合材料,所述的TiAl基复合材料按原子百分含量含有:42%Al、0.5%B、1.5%Cr、5%Nb、0.2%Ta,余量为Ti和不可避免的杂质。Preferably, the present invention provides a third TiAl-based composite material, the TiAl-based composite material contains by atomic percentage: 42% Al, 0.5% B, 1.5% Cr, 5% Nb, 0.2% Ta, the balance for Ti and inevitable impurities.

另一方面,本发明提供一种TiAl复合材料的制备方法,步骤如下:On the other hand, the present invention provides a kind of preparation method of TiAl composite material, and the steps are as follows:

步骤一:铸锭熔炼:按照成分配比将原材料混合均匀后,在压力机上压制成电极块;进行三次真空自耗熔炼;获得直径为Φ180mm~Φ300mm的复合材料铸锭;Step 1: Ingot smelting: After mixing the raw materials uniformly according to the composition ratio, press it into an electrode block on a press; carry out three vacuum consumable smelting; obtain a composite material ingot with a diameter of Φ180mm~Φ300mm;

步骤二:挤压变形:将所获得的复合材料铸锭进行包套挤压变形,包套与所述复合材料铸锭之间添加隔热材料,挤压变形后将复合材料棒材空冷或炉冷至室温;Step 2: Extrusion deformation: The obtained composite material ingot is subjected to wrapping and extruding deformation, heat insulating material is added between the wrapping and the composite material ingot, and the composite material bar is air-cooled or furnaced after the extrusion deformation. cool to room temperature;

步骤三:均匀化退火:将上一步得到的材料加热到1050℃~1200℃,保温6~48小时,而后冷却到室温或者直接升温到固溶温度;Step 3: Homogenization annealing: heating the material obtained in the previous step to 1050°C to 1200°C, keeping the temperature for 6 to 48 hours, and then cooling to room temperature or directly heating up to the solution temperature;

步骤四:固溶热处理:将均匀化退火后的材料进行两相区或者单相区固溶热处理;Step 4: Solution heat treatment: the material after homogenization annealing is subjected to solution heat treatment in a two-phase region or a single-phase region;

步骤五:时效热处理:将经过固溶热处理后的材料加热到850℃~950℃,保温2~8小时,而后炉冷到室温。Step 5: Aging heat treatment: The material after solution heat treatment is heated to 850°C to 950°C, kept for 2 to 8 hours, and then cooled to room temperature in the furnace.

所述步骤一中参数:熔炼真空度低于5Pa,熔炼电流为3kA~6kA,熔炼电压为23~27V。The parameters in the first step: the smelting vacuum degree is lower than 5Pa, the smelting current is 3kA-6kA, and the smelting voltage is 23-27V.

所述步骤二参数:包套材料采用不锈钢,挤压变形温度范围1100℃~1250℃,挤压比大于6:1。The parameters of the second step: the sheath material is stainless steel, the extrusion deformation temperature is in the range of 1100°C to 1250°C, and the extrusion ratio is greater than 6:1.

所述的两相区固溶热处理为γ+α两相区固溶热处理,具体如下:The solid solution heat treatment in the two-phase region is the solid solution heat treatment in the γ+α two-phase region, and the details are as follows:

热处理温度为1200℃~Tα-15℃,其中Tα为γ→α相变温度;保温0.5~6小时,而后空冷或炉冷到室温。The heat treatment temperature is 1200℃~T α -15℃, where T α is the γ→α phase transition temperature; the temperature is kept for 0.5 to 6 hours, and then air-cooled or furnace cooled to room temperature.

所述的单相区固溶热处理为α单相区固溶热处理,具体如下:The single-phase region solid solution heat treatment is the α single-phase region solid solution heat treatment, and the details are as follows:

热处理温度为Tα+5℃~Tα+20℃,其中Tα为γ→α相变温度;保温5min~2小时,而后空冷、炉冷或者油淬到室温The heat treatment temperature is T α +5℃~T α +20℃, where T α is the γ→α phase transition temperature; keep for 5min~2 hours, and then air cooling, furnace cooling or oil quenching to room temperature

所述步骤三之前还包含等温锻造的步骤,具体为:The step of isothermal forging is also included before the third step, specifically:

将复合材料棒材加热到1050℃~1250℃,锻造模具加热到900℃~1150℃,锻造变形速率为0.001s-1~0.05s-1,锻造变形量≥40%,锻造变形后将锻件空冷或炉冷至室温。The composite material bar is heated to 1050℃~1250℃, the forging die is heated to 900℃~1150℃, the forging deformation rate is 0.001s -1 ~ 0.05s -1 , the forging deformation is ≥40%, and the forging is air-cooled after forging deformation Or oven cool to room temperature.

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

(1)TiAl基复合材料(TiB2/TiAl)的增强体TiB2晶须是由共晶反应从液相中直接原位生成的,TiB2晶须增强体与TiAl合金基体之间不存在界面反应问题。(1) The reinforcement of TiAl matrix composites (TiB 2 /TiAl) TiB 2 whiskers are directly generated in situ from the liquid phase by the eutectic reaction, and there is no interface between the TiB 2 whisker reinforcement and the TiAl alloy matrix response question.

(2)原位自生成的TiB2晶须能显著细化铸造组织,有利于改善TiB2/TiAl复合材料的热加工工艺性能。(2) The in-situ self-generated TiB 2 whiskers can significantly refine the casting structure, which is beneficial to improve the thermal processing performance of TiB 2 /TiAl composites.

(3)TiB2/TiAl复合材料经过热机械处理后,细长的TiB2晶须破碎成短晶须,弥散分布的TiB2短晶须能够抑制晶粒长大,改善塑性,并提高强度。(3) After the thermal mechanical treatment of TiB 2 /TiAl composites, the slender TiB 2 whiskers are broken into short whiskers, and the dispersed short TiB 2 whiskers can inhibit the grain growth, improve the plasticity, and increase the strength.

以往研究者通常将B作为微量元素添加到TiAl合金中,添加量小于0.2at%,因为担心大量的TiB2颗粒会导致室温塑性降低。由于这些TiAl合金中B的添加量偏低,没有足够量的TiB2相,强化效果不明显,因此无法有效提高TiAl合金的强度。我们的研究表明,B含量在0.5at%以上,可以降低TiAl合金铸锭晶粒度一个数量级,而且控制好B含量的上限,可以使TiB2通过共晶反应生长成晶须状,而不会生长成粗大的颗粒状TiB2,这种细长的晶须状TiB2相经过后续的热加工,将破碎成短晶须,可显著提高TiB2/TiAl复合材料高温强度,同时还有良好的室温塑性,因此有良好的工程应用前景。In the past, researchers usually added B as a trace element to TiAl alloys, and the addition amount was less than 0.2 at%, because it was worried that a large number of TiB particles would lead to the reduction of room temperature plasticity. Since the addition amount of B in these TiAl alloys is relatively low, there is not enough TiB 2 phase, and the strengthening effect is not obvious, so the strength of TiAl alloys cannot be effectively improved. Our research shows that when the B content is above 0.5at%, the grain size of TiAl alloy ingot can be reduced by an order of magnitude, and the upper limit of the B content can be controlled well, which can make TiB2 grow into whiskers through eutectic reaction, without It grows into coarse granular TiB 2 , and this slender, whisker-like TiB 2 phase will be broken into short whiskers after subsequent thermal processing, which can significantly improve the high temperature strength of TiB 2 /TiAl composites, and also has good properties. Plasticity at room temperature, so it has good engineering application prospects.

附图说明Description of drawings

为了更清楚地说明本发明实施的技术方案,下面将对本发明的实例中需要使用的附图作简单的解释。显而易见,下面所描述的附图仅仅是本发明的一些实施例,对于本领域的技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他的附图。In order to illustrate the technical solutions implemented by the present invention more clearly, the following will briefly explain the accompanying drawings that need to be used in the examples of the present invention. Obviously, the drawings described below are only some embodiments of the present invention, and for those skilled in the art, other drawings can also be obtained from these drawings without creative effort.

图1为TiB2/TiAl复合材料中的TiB2晶须TEM形貌;Figure 1 shows the TEM morphology of TiB 2 whiskers in TiB 2 /TiAl composites;

图2为B含量对TiAl合金晶粒尺寸的影响;Figure 2 shows the effect of B content on the grain size of TiAl alloy;

图3为实施例1经热挤压变形后复合材料中的TiB2短晶须。Figure 3 shows the TiB 2 short whiskers in the composite material after hot extrusion deformation in Example 1.

具体实施方式Detailed ways

为使本发明实施例的目的、技术方案和优点更加清楚,下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述。显然,所描述的实施例是本发明的一部分实施例,而不是全部实施例。基于本发明中的实施例,本领域的普通技术人员在没有做出创造性劳动的前提下,所获得的所有其他实施例,都属于本发明保护的范围。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be described clearly and completely below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are some, but not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the protection scope of the present invention.

下面将详细描述本发明实施例的各个方面的特征。在下面的详细描述中,提出了许多具体的细节,以便对本发明的全面理解。但是,对于本领域的普通技术人员来说,很明显的是,本发明也可以在不需要这些具体细节的情况下就可以实施。下面对实施例的描述仅仅是为了通过示出本发明的示例对本发明更好的理解。本发明不限于下面所提供的任何具体设置和方法,而是覆盖了不脱离本发明精神的前提下所覆盖的所有的产品结构、方法的任何改进、替换等。The features of various aspects of the embodiments of the present invention will be described in detail below. In the following detailed description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. However, it will be apparent to one of ordinary skill in the art that the present invention may be practiced without these specific details. The following description of the embodiments is only for a better understanding of the present invention by illustrating examples of the invention. The present invention is not limited to any specific arrangements and methods provided below, but covers all product structures, any improvements, substitutions, and the like of methods covered without departing from the spirit of the present invention.

在各个附图和下面的描述中,没有示出公知的结构和技术,以避免对本发明造成不必要的模糊。In the various drawings and the following description, well-known structures and techniques have not been shown in order to avoid unnecessarily obscuring the present invention.

实施例1:Example 1:

本发明在TiAl合金中添加合适量的B元素,通过铸锭熔炼在TiAl合金基体上原位自生成细长的TiB2晶须,并通过后续的热机械处理,制备成TiB2/TiAl复合材料。复合材料中的TiB2相是以液态金属凝固过程中L→β+TiB2和L+β→α+TiB2共晶反应与基体原位耦合生长的细长次生TiB2晶须(见图1所示),晶须的宽度约0.5μm,长度几十微米。In the present invention, an appropriate amount of B element is added to the TiAl alloy, and slender TiB 2 whiskers are generated in-situ on the TiAl alloy matrix by ingot smelting, and the TiB 2 /TiAl composite material is prepared by subsequent thermomechanical treatment. . The TiB 2 phase in the composite is composed of elongated secondary TiB 2 whiskers grown in situ coupled with the matrix by L→β+TiB 2 and L+β→α+TiB 2 eutectic reactions during solidification of liquid metal (see Fig. 1), the whiskers have a width of about 0.5 μm and a length of several tens of microns.

本发明TiB2/TiAl复合材料可以采用如下方式生产:The TiB 2 /TiAl composite material of the present invention can be produced in the following manner:

本实施例1的TiB2/TiAl复合材料通过下述步骤制备:The TiB 2 /TiAl composite material of this Example 1 was prepared by the following steps:

TiB2/TiAl复合材料原材料采用了零级海绵钛、A00级高纯铝、金属Cr、Al-Nb中间合金、Al-Ta中间合金、Al-Si中间合金和Al-Ti-B中间合金。按原子百分含量含有:45.5%Al、0.5%B、1.5%Cr、4%Nb、0.2%Ta、0.2%Si,其余为Ti。The raw materials of TiB 2 /TiAl composite material are zero-grade sponge titanium, A00-grade high-purity aluminum, metal Cr, Al-Nb master alloy, Al-Ta master alloy, Al-Si master alloy and Al-Ti-B master alloy. According to atomic percentage, it contains: 45.5% Al, 0.5% B, 1.5% Cr, 4% Nb, 0.2% Ta, 0.2% Si, and the rest is Ti.

将原材料混合均匀后,在压力机上压制成电极块。电极块焊接后,在真空自耗熔炼炉内进行三次熔炼,熔炼真空度低于5Pa,熔炼电流根据锭型尺寸控制在3kA~6kA范围内,熔炼电压23~25V,三次熔炼后获得直径Φ220mm铸锭。After the raw materials are mixed uniformly, they are pressed into electrode blocks on a press. After the electrode block is welded, three times of melting are carried out in the vacuum consumable melting furnace. The melting vacuum degree is lower than 5Pa. ingot.

将TiB2/TiAl复合材料铸锭进行包套挤压变形,包套材采用不锈钢,包套与TiB2/TiAl复合材料铸锭之间添加隔热材料,挤压温度范围1200℃~1250℃,挤压比10:1,挤压变形后将棒材空冷至室温。经过热挤压变形后,TiB2/TiAl复合材料中的TiB2相破碎成了细小弥散的短晶须,平均长度15μm,并沿挤压变形方向排列,见附图3所示。The TiB 2 /TiAl composite material ingot is extruded and deformed by wrapping, the wrapping material is made of stainless steel, and heat insulating material is added between the wrapping and the TiB 2 /TiAl composite material ingot, and the extrusion temperature range is 1200℃~1250℃. The extrusion ratio is 10:1, and the bar is air-cooled to room temperature after extrusion deformation. After hot extrusion deformation, the TiB 2 phase in the TiB 2 /TiAl composite material was broken into fine and dispersed short whiskers with an average length of 15 μm, which were arranged along the extrusion deformation direction, as shown in Figure 3.

将挤压棒材下料后进行等温模锻,坯料加热到1150℃,锻造模具加热到1000℃,锻造变形速率控制在0.001s-1~0.01s-1范围内,锻造变形量50%,锻造变形后将锻件空冷至室温。The extruded bar is blanked and then subjected to isothermal die forging, the billet is heated to 1150 °C, the forging die is heated to 1000 °C, the forging deformation rate is controlled within the range of 0.001s -1 ~ 0.01s -1 , the forging deformation is 50%, and the forging After deformation, the forgings are air-cooled to room temperature.

将TiB2/TiAl复合材料挤压棒材或等温锻件进行1150℃/16小时/空冷的均匀化退火处理;而后进行1300℃/0.5小时/空冷的固溶处理;最后进行900℃/6小时炉冷的时效热处理。The TiB 2 /TiAl composite extruded bars or isothermal forgings are subjected to homogenization annealing treatment at 1150°C/16 hours/air cooling; then solution treatment at 1300°C/0.5 hours/air cooling; and finally a furnace at 900°C/6 hours Cold aging heat treatment.

表1和表2分别为实施例1的室温和850℃拉伸性能。经过热机械处理的TiB2/TiAl复合材料的室温塑性可达2%以上,室温屈服强度达600MPa以上,850℃屈服强度仍保持在400MPa以上。Table 1 and Table 2 are the room temperature and 850°C tensile properties of Example 1, respectively. The room temperature plasticity of TiB 2 /TiAl composites after thermomechanical treatment can reach more than 2%, the room temperature yield strength is more than 600MPa, and the yield strength at 850℃ remains above 400MPa.

表1实施例1的室温拉伸性能Table 1 Room temperature tensile properties of Example 1

Figure BDA0002234171570000061
Figure BDA0002234171570000061

表2实施例1的850℃拉伸性能Table 2 Tensile properties at 850°C of Example 1

Figure BDA0002234171570000062
Figure BDA0002234171570000062

实施例2:Example 2:

实施例2的TiB2/TiAl复合材料通过下述步骤制备:The TiB 2 /TiAl composite material of Example 2 was prepared by the following steps:

实施例2的TiB2/TiAl复合材料原材料采用了零级海绵钛、A00级高纯铝、金属Cr、Al-Nb中间合金和TiB2粉末。按原子百分含量含有:44%Al、0.8%B、1%Cr、4%Nb,0.2%Ta,其余为Ti。The raw materials of the TiB 2 /TiAl composite material in Example 2 are zero-grade sponge titanium, A00-grade high-purity aluminum, metal Cr, Al-Nb master alloy and TiB 2 powder. By atomic percentage, it contains: 44% Al, 0.8% B, 1% Cr, 4% Nb, 0.2% Ta, and the rest is Ti.

将原材料混合均匀后,在压力机上压制成电极块。电极块焊接后,在真空自耗熔炼炉内进行三次熔炼,熔炼真空度低于5Pa,熔炼电流根据锭型尺寸控制在3kA~6kA范围内,熔炼电压23~25V,三次熔炼后获得直径Φ220mm铸锭。After the raw materials are mixed uniformly, they are pressed into electrode blocks on a press. After the electrode block is welded, three times of melting are carried out in the vacuum consumable melting furnace. The melting vacuum degree is lower than 5Pa. ingot.

将TiB2/TiAl复合材料铸锭进行包套挤压变形,包套材采用不锈钢,包套与TiB2/TiAl复合材料铸锭之间添加隔热材料,挤压温度范围1200℃~1250℃,挤压比10:1,挤压变形后将棒材空冷至室温。The TiB 2 /TiAl composite material ingot is extruded and deformed by wrapping, the wrapping material is made of stainless steel, and heat insulating material is added between the wrapping and the TiB 2 /TiAl composite material ingot, and the extrusion temperature range is 1200℃~1250℃. The extrusion ratio is 10:1, and the bar is air-cooled to room temperature after extrusion deformation.

将TiB2/TiAl复合材料挤压棒材进行1150℃/16小时/空冷的均匀化退火处理;而后进行1280℃/0.5小时/空冷的固溶处理;最后进行900℃/6小时炉冷的时效热处理。The TiB 2 /TiAl composite extruded bar was subjected to homogenization annealing treatment at 1150°C/16 hours/air cooling; then solution treatment at 1280°C/0.5 hours/air cooling; and finally furnace cooling at 900°C/6 hours aging heat treatment.

表3和表4分别为实施例2的室温和850℃拉伸性能。经过热机械处理的TiB2/TiAl复合材料的室温塑性可达2%,室温屈服强度达550MPa以上,850℃屈服强度仍保持在400MPa以上。Tables 3 and 4 are the room temperature and 850°C tensile properties of Example 2, respectively. The room temperature plasticity of TiB 2 /TiAl composites after thermomechanical treatment can reach 2%, the room temperature yield strength is above 550MPa, and the yield strength at 850℃ remains above 400MPa.

表3实施例2的室温拉伸性能Table 3 Room temperature tensile properties of Example 2

Figure BDA0002234171570000071
Figure BDA0002234171570000071

表4实施例2的850℃拉伸性能Table 4 Tensile properties at 850°C of Example 2

Figure BDA0002234171570000072
Figure BDA0002234171570000072

实施例3:Example 3:

实施例3的TiB2/TiAl复合材料通过下述步骤制备:The TiB 2 /TiAl composite material of Example 3 was prepared by the following steps:

实施例3的TiB2/TiAl复合材料原材料采用了零级海绵钛、A00级高纯铝、金属Cr、Al-Nb中间合金和TiB2粉末。按原子百分含量含有:42%Al、0.5%B、1.5%Cr、5%Nb,0.2%Ta,其余为Ti。The raw materials of the TiB 2 /TiAl composite material in Example 3 are zero-grade titanium sponge, A00-grade high-purity aluminum, metal Cr, Al-Nb master alloy and TiB 2 powder. According to atomic percentage, it contains: 42% Al, 0.5% B, 1.5% Cr, 5% Nb, 0.2% Ta, and the rest is Ti.

将原材料混合均匀后,在压力机上压制成电极块。电极块焊接后,在真空自耗熔炼炉内进行三次熔炼,熔炼真空度低于5Pa,熔炼电流根据锭型尺寸控制在3kA~6kA范围内,熔炼电压23~25V,三次熔炼后获得直径Φ300mm铸锭。After the raw materials are mixed uniformly, they are pressed into electrode blocks on a press. After the electrode block is welded, three times of melting are carried out in the vacuum consumable melting furnace. The melting vacuum degree is lower than 5Pa. The melting current is controlled within the range of 3kA~6kA according to the size of the ingot, and the melting voltage is 23~25V. ingot.

将TiB2/TiAl复合材料铸锭进行包套挤压变形,包套材采用不锈钢,包套与TiB2/TiAl复合材料铸锭之间添加隔热材料,挤压温度范围1150℃~1200℃,挤压比10:1,挤压变形后将棒材空冷至室温。The TiB 2 /TiAl composite ingot is extruded and deformed by wrapping. The wrapping material is made of stainless steel. Insulation material is added between the wrapping and the TiB 2 /TiAl composite ingot. The extrusion temperature ranges from 1150°C to 1200°C. The extrusion ratio is 10:1, and the bar is air-cooled to room temperature after extrusion deformation.

将TiB2/TiAl复合材料挤压棒材进行1100℃/16小时/空冷的均匀化退火处理;而后进行1210℃/0.5小时/空冷的固溶处理;最后进行900℃/6小时炉冷的时效热处理。The TiB 2 /TiAl composite extruded rod was subjected to homogenization annealing treatment at 1100°C/16 hours/air cooling; then solution treatment at 1210°C/0.5 hours/air cooling; and finally, furnace cooling at 900°C/6 hours for aging heat treatment.

表5和表6分别为实施例2的室温和850℃拉伸性能。经过热机械处理的TiB2/TiAl复合材料的室温塑性可达2%,室温屈服强度达800MPa以上,850℃屈服强度仍保持在500MPa以上。Table 5 and Table 6 are the room temperature and 850°C tensile properties of Example 2, respectively. The room temperature plasticity of TiB 2 /TiAl composites after thermomechanical treatment can reach 2%, the room temperature yield strength is above 800MPa, and the yield strength at 850℃ is still above 500MPa.

表5实施例3的室温拉伸性能Table 5 Room temperature tensile properties of Example 3

Figure BDA0002234171570000081
Figure BDA0002234171570000081

表6实施例3的850℃拉伸性能Table 6 Tensile properties at 850°C of Example 3

本发明采用铸锭冶金的方法制备原位自生成TiAl基复合材料具有如下优点:The present invention adopts the method of ingot metallurgy to prepare the in-situ self-generated TiAl-based composite material and has the following advantages:

(1)TiAl基复合材料(TiB2/TiAl)的增强体TiB2晶须是由共晶反应从液相中直接原位生成的,TiB2晶须增强体与TiAl合金基体之间不存在界面反应问题。如图1所示,TEM照片显示TiB2晶须与TiAl合金基体界面结合良好,没有发生界面反应。(1) The reinforcement of TiAl matrix composites (TiB 2 /TiAl) TiB 2 whiskers are directly generated in situ from the liquid phase by the eutectic reaction, and there is no interface between the TiB 2 whisker reinforcement and the TiAl alloy matrix response question. As shown in Fig. 1 , the TEM image shows that the TiB whiskers are well bonded to the TiAl alloy matrix interface, and no interfacial reaction occurs.

(2)原位自生成的TiB2晶须能显著细化铸造组织,有利于改善TiB2/TiAl复合材料的热加工工艺性能。如图2所示,当B含量达0.5at%,TiB2/TiAl复合材料的晶粒尺寸比不添加B的TiAl合金晶粒尺寸下降一个数量级。(2) The in-situ self-generated TiB 2 whiskers can significantly refine the casting structure, which is beneficial to improve the thermal processing performance of TiB 2 /TiAl composites. As shown in Fig. 2, when the B content reaches 0.5 at%, the grain size of the TiB 2 /TiAl composite decreases by an order of magnitude compared with that of the TiAl alloy without B addition.

(3)TiB2/TiAl复合材料经过热机械处理后,细长的TiB2晶须破碎成短晶须,弥散分布的TiB2短晶须能够抑制晶粒长大,改善塑性,并提高强度。(3) After the thermal mechanical treatment of TiB 2 /TiAl composites, the slender TiB 2 whiskers are broken into short whiskers, and the dispersed short TiB 2 whiskers can inhibit the grain growth, improve the plasticity, and increase the strength.

该复合材料具有优异高温强度和高温持久性能,同时还有较好的室温塑性。TiB2/TiAl复合材料的使用温度可达850℃,可用于制造航空发动机叶片、机匣、扩压器等零件以及高超音速飞行器耐热部件The composite material has excellent high temperature strength and high temperature durability, as well as good room temperature plasticity. The working temperature of TiB 2 /TiAl composite material can reach 850 ℃, which can be used to manufacture parts such as aero-engine blades, casings, diffusers, and heat-resistant parts of hypersonic aircraft

最后应该说明的是:以上实施例仅用以说明本发明的技术方案,但本发明的保护范围并不局限于此,任何熟悉本领域的技术人员在本发明揭露的技术范围内,可以轻易想到各种等效的修改或者替换,这些修改或者替换都应该涵盖在本发明的保护范围之内。Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, but the protection scope of the present invention is not limited to this. Various equivalent modifications or substitutions should be included within the protection scope of the present invention.

Claims (10)

1. A TiAl-based composite material, characterized in that: the TiAl-based composite material comprises the following components in percentage by atom: 0.5 to 1.5 percent of B, 42 to 45.5 percent of Al, 1 to 2 percent of Cr, 3 to 6 percent of Nb, 0.1 to 0.5 percent of Ta, 0 to 0.2 percent of Si, 0 to 2 percent of C, and the balance of Ti and inevitable impurities, wherein the oxygen content is less than or equal to 0.2 percent by weight, the nitrogen content is less than or equal to 0.03 percent by weight, and the hydrogen content is less than or equal to 0.02 percent by weight;
the elastic modulus E of the TiAl-based composite material is more than or equal to 150 GPa;
the TiAl-based composite material has the reinforcing body of TiAl-based composite material which is TiB distributed in a dispersed way2Short whiskers, wherein the length of the whiskers is less than or equal to 30 microns.
2. The TiAl-based composite material according to claim 1, characterized in that: the TiAl-based composite material comprises the following components in percentage by atom: 45.5% of Al, 0.5% of B, 1.5% of Cr, 4% of Nb, 0.2% of Ta, 0.2% of Si, and the balance of Ti and inevitable impurities.
3. The TiAl-based composite material according to claim 1, characterized in that: the TiAl-based composite material comprises the following components in percentage by atom: 44% of Al, 0.8% of B, 1% of Cr, 4% of Nb, 0.2% of Ta, and the balance of Ti and inevitable impurities.
4. The TiAl-based composite material according to claim 1, characterized in that: the TiAl-based composite material comprises the following components in percentage by atom: 42% of Al, 0.5% of B, 1.5% of Cr, 5% of Nb, 0.2% of Ta, and the balance of Ti and inevitable impurities.
5. A thermal mechanical treatment method of a TiAl-based composite material is characterized in that: the method of thermomechanical treatment using the TiAl-based composite material according to claim 1, comprising the steps of:
the method comprises the following steps: smelting of cast ingots: uniformly mixing the raw materials according to the component ratio, and pressing the mixture into an electrode block on a press machine; carrying out three times of vacuum consumable melting; obtaining a composite material ingot with the diameter of phi 180 mm-phi 300 mm;
step two: extrusion deformation: performing sheath extrusion deformation on the obtained composite material cast ingot, adding a heat insulating material between the sheath and the composite material cast ingot, and performing air cooling or furnace cooling on the composite material bar to room temperature after the extrusion deformation;
step three: homogenizing and annealing: heating the material obtained in the last step to 1050-1200 ℃, preserving heat for 6-48 hours, and then cooling to room temperature or directly heating to a solid solution temperature;
step four: solution heat treatment: carrying out solution heat treatment on the homogenized and annealed material in a two-phase region or a single-phase region;
step five: aging heat treatment: and heating the material subjected to the solution heat treatment to 850-950 ℃, preserving the heat for 2-8 hours, and then cooling the material to room temperature.
6. The method for thermomechanical treatment of TiAl-based composite materials according to claim 5, characterized in that: parameters in the first step are set as follows:
the smelting vacuum degree is lower than 5Pa, the smelting current is 3 kA-6 kA, and the smelting voltage is 23-27V.
7. The method for thermomechanical treatment of TiAl-based composite materials according to claim 5, characterized in that: and in the second step, the jacket material is stainless steel, the extrusion deformation temperature range is 1100-1250 ℃, and the extrusion ratio is more than 6: 1.
8. The method for thermomechanical treatment of TiAl-based composite materials according to claim 5, characterized in that: the two-phase region solution heat treatment in the fourth step is a gamma + alpha two-phase region solution heat treatment, which comprises the following specific steps:
the heat treatment temperature is 1200-Tα-15 ℃ of which TαIs gamma → alpha phase transition temperature; keeping the temperature for 0.5 to 6 hours, andand then air cooling or furnace cooling is carried out to the room temperature.
9. The method for thermomechanical treatment of TiAl-based composite materials according to claim 5, characterized in that: in the fourth step, the single-phase zone solution heat treatment is alpha single-phase zone solution heat treatment, which comprises the following specific steps:
heat treatment temperature Tα+5℃~Tα+20 ℃ where T isαIs gamma → alpha phase transition temperature; preserving the temperature for 5min to 2 hours, and then air cooling, furnace cooling or oil quenching to room temperature.
10. The method for thermomechanical treatment of TiAl-based composite materials according to claim 5, characterized in that: before the third step, isothermal forging is also included, specifically:
heating the composite material bar to 1050-1250 ℃, heating the forging die to 900-1150 ℃, and forging the deformation rate of 0.001s-1~0.05s-1And the forging deformation is more than or equal to 40 percent, and the forging is cooled in air or furnace to room temperature after the forging deformation.
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CN114150181A (en) * 2021-11-25 2022-03-08 南京理工大学 A kind of low-cost easy-deformable light-weight high-strength TiAl alloy and preparation method thereof
CN115109965A (en) * 2022-06-28 2022-09-27 中国航发北京航空材料研究院 A kind of high plasticity polycrystalline TiAl alloy and preparation method thereof
CN115505787A (en) * 2022-09-30 2022-12-23 中国航发北京航空材料研究院 A light-weight and high-temperature-resistant titanium-based multi-principal composite material
CN116274452A (en) * 2023-03-31 2023-06-23 中国科学院金属研究所 A deformed superalloy rod and its preparation method
CN117802433A (en) * 2023-12-29 2024-04-02 北京钢研高纳科技股份有限公司 TiAl-based alloy square billet bar and preparation method and application thereof
CN118080747A (en) * 2023-11-20 2024-05-28 北京科技大学 Ultrahigh-temperature plastic forming method for TiAl alloy blade

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CN113528890B (en) * 2020-04-16 2022-09-30 中国科学院金属研究所 High-oxidation-resistance and high-plasticity deformed TiAl-based alloy and preparation process thereof
CN113528890A (en) * 2020-04-16 2021-10-22 中国科学院金属研究所 Deformed TiAl-based alloy with high oxidation resistance and high plasticity and its preparation process
CN112159913B (en) * 2020-08-25 2022-03-01 中国石油天然气集团有限公司 135 ksi-grade titanium alloy, titanium alloy drill rod and preparation method thereof
CN112159913A (en) * 2020-08-25 2021-01-01 中国石油天然气集团有限公司 135 ksi-grade titanium alloy, titanium alloy drill rod and preparation method thereof
CN112746232A (en) * 2020-12-28 2021-05-04 西北工业大学 Method for improving strong plasticity of beta-type gamma-TiAl alloy
CN112746232B (en) * 2020-12-28 2021-12-28 西北工业大学 A method for improving the strength and plasticity of β-type γ-TiAl alloy
CN113755769A (en) * 2021-08-13 2021-12-07 上海交通大学 A kind of high strength and high toughness aluminum matrix composite material and heat treatment method
CN114150181A (en) * 2021-11-25 2022-03-08 南京理工大学 A kind of low-cost easy-deformable light-weight high-strength TiAl alloy and preparation method thereof
CN115109965A (en) * 2022-06-28 2022-09-27 中国航发北京航空材料研究院 A kind of high plasticity polycrystalline TiAl alloy and preparation method thereof
CN115109965B (en) * 2022-06-28 2023-09-15 中国航发北京航空材料研究院 High-plasticity polycrystalline TiAl alloy and preparation method thereof
CN115505787A (en) * 2022-09-30 2022-12-23 中国航发北京航空材料研究院 A light-weight and high-temperature-resistant titanium-based multi-principal composite material
CN116274452A (en) * 2023-03-31 2023-06-23 中国科学院金属研究所 A deformed superalloy rod and its preparation method
CN118080747A (en) * 2023-11-20 2024-05-28 北京科技大学 Ultrahigh-temperature plastic forming method for TiAl alloy blade
CN117802433A (en) * 2023-12-29 2024-04-02 北京钢研高纳科技股份有限公司 TiAl-based alloy square billet bar and preparation method and application thereof

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