CN117966052A - Preparation method of titanium-based composite material with high strength and toughness and service performance at 700 DEG C - Google Patents
Preparation method of titanium-based composite material with high strength and toughness and service performance at 700 DEG C Download PDFInfo
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Abstract
Description
技术领域Technical Field
本发明涉及一种兼具高强韧与700℃服役性能的钛基复合材料制备方法,属于钛合金及其复合材料技术领域。The invention relates to a method for preparing a titanium-based composite material with high strength and toughness and 700°C service performance, belonging to the technical field of titanium alloys and composite materials thereof.
背景技术Background technique
为满足未来航空航天飞行器对结构减重和性能提升的双重需求,尤其是对轻质结构关键部件在室温和高温条件下高韧性和高温服役性能的紧迫需求。高温钛合金作为现代航空发动机的关键材料,被广泛应用于航空发动机的叶片、机盘、机匣等部件,以降低发动机重量,提高飞机的推重比,从而显著提升了航空发动机的服役性能。然而,随着飞行器使用温度的升高,对高温钛合金的使役性能提出了更高的要求。同时,飞行器的服役条件变得更加复杂,对高温钛合金的使役性能需求也不再局限于单一的性能指标,而是期望其在室温和高温条件下具备卓越的综合性能。In order to meet the dual needs of future aerospace vehicles for structural weight reduction and performance improvement, especially the urgent need for high toughness and high-temperature service performance of key lightweight structural components at room temperature and high temperature conditions. As a key material for modern aircraft engines, high-temperature titanium alloys are widely used in aircraft engine blades, disks, casings and other components to reduce engine weight and improve the thrust-to-weight ratio of aircraft, thereby significantly improving the service performance of aircraft engines. However, with the increase in the operating temperature of aircraft, higher requirements are placed on the service performance of high-temperature titanium alloys. At the same time, the service conditions of aircraft have become more complex, and the service performance requirements of high-temperature titanium alloys are no longer limited to a single performance indicator, but are expected to have excellent comprehensive performance at room temperature and high temperature conditions.
为了进一步提升钛合金的综合性能,目前研究的焦点主要集中在通过复合化的方式实现材料的高温强度提升。然而,过去的钛基复合材料存在一些问题,如增强相类型单一、忽视对基体钛合金微观组织的设计与调控。因此,目前市场上开发的商业高温钛合金在室温强度方面相对不足,且仍然存在室温强度-塑/韧性的倒置问题。更为关键的是,这些材料在650℃以上的高温条件下性能不足,迫切需要开发一种使役温度在700℃以上,并且同时具备卓越室温强塑性的新型钛合金及其复合材料。In order to further improve the comprehensive performance of titanium alloys, the current research focus is mainly on improving the high-temperature strength of materials through composite methods. However, there are some problems with titanium-based composite materials in the past, such as the single type of reinforcing phase and the neglect of the design and regulation of the microstructure of the matrix titanium alloy. Therefore, the commercial high-temperature titanium alloys currently developed on the market are relatively insufficient in terms of room temperature strength, and there is still an inversion problem of room temperature strength-plasticity/toughness. More importantly, these materials have insufficient performance under high temperature conditions above 650°C. There is an urgent need to develop a new type of titanium alloy and its composite materials with a service temperature above 700°C and excellent room temperature strength and plasticity.
发明内容Summary of the invention
本发明为解决现有高温钛基复合材料研究中室温强塑性匹配与高温强度提升难以兼具的瓶颈问题,进而提出一种兼具高强韧与700℃服役性能的钛基复合材料制备方法。The present invention aims to solve the bottleneck problem that it is difficult to achieve both room temperature strength and plasticity matching and high temperature strength improvement in existing high temperature titanium-based composite material research, and further proposes a method for preparing a titanium-based composite material with both high strength and toughness and 700°C service performance.
本发明为解决上述问题采取的技术方案是:本发明包括下列步骤:The technical solution adopted by the present invention to solve the above-mentioned problem is: the present invention comprises the following steps:
步骤1、根据设计的增强相的含量,计算外加粉体M中的各强化粉体在原料粉体中的含量,以确定TC25G合金粉体和各强化粉体的质量比;Step 1: Calculate the content of each strengthening powder in the added powder M in the raw material powder according to the designed strengthening phase content, so as to determine the mass ratio of the TC25G alloy powder and each strengthening powder;
步骤2、按照设计的质量比称取TC25G合金粉体与外加粉体,并进行球磨混合,使粉体混合均匀,获得复合粉体;Step 2, weighing TC25G alloy powder and external powder according to the designed mass ratio, and mixing them by ball milling to make the powders evenly mixed to obtain composite powder;
步骤3、将获得的所述复合粉体进行热压烧结,并进行原位自生反应制备获得块体复合材料;Step 3, hot pressing and sintering the obtained composite powder, and performing an in-situ autogenous reaction to prepare a bulk composite material;
步骤4、将获得的所述块体复合材料进行热挤压,获得兼具室温强塑性与服役性的钛基复合材料。Step 4: hot-extrude the obtained block composite material to obtain a titanium-based composite material with both room temperature strength and plasticity and serviceability.
进一步的,步骤1中所述外加粉体包括原始β晶界强化粉体、α/β相界强化粉体以及基体强化粉体。Furthermore, the added powder in step 1 includes original β grain boundary strengthening powder, α/β phase boundary strengthening powder and matrix strengthening powder.
进一步的,所述原始β晶界强化粉体在所述复合粉体中所占质量分数为0.05-5%,所述原始β晶界强化粉体包括B粉、TiB2粉、Y粉以及La粉中至少一种粉体,且所述原始β晶界强化粉体粒径为0.05-10μm。Furthermore, the mass fraction of the original β grain boundary strengthening powder in the composite powder is 0.05-5%, the original β grain boundary strengthening powder includes at least one of B powder, TiB2 powder, Y powder and La powder, and the particle size of the original β grain boundary strengthening powder is 0.05-10μm.
进一步的,步骤3中,通过所述原位自生反应在原始β晶界处生成TiB、Y2O3和La2O3中至少一种增强相。Furthermore, in step 3, at least one reinforcing phase of TiB, Y 2 O 3 and La 2 O 3 is generated at the original β grain boundary through the in-situ autogenous reaction.
进一步的,所述α/β相界强化粉体在所述复合粉体中所占质量分数为0.05-3%;所述α/β相界强化粉体包括Si粉,且所述α/β相界强化粉体的粒径为0.05-5μm。Furthermore, the mass fraction of the α/β phase boundary strengthening powder in the composite powder is 0.05-3%; the α/β phase boundary strengthening powder includes Si powder, and the particle size of the α/β phase boundary strengthening powder is 0.05-5 μm.
进一步的,步骤3中,通过所述原位自生反应在α/β相界面处生成(Ti,Zr)5Si3和(Ti,Zr)6Si3中至少一种增强相,且所述增强相的尺寸为0.01-5μm。Furthermore, in step 3, at least one reinforcing phase of (Ti, Zr) 5 Si 3 and (Ti, Zr) 6 Si 3 is generated at the α/β phase interface through the in-situ autogenous reaction, and the size of the reinforcing phase is 0.01-5 μm.
进一步的,所述基体强化粉体在所述复合粉体中所占质量分数为0.05-5%,所述基体强化粉体包括Ta粉、Mo粉以及W粉中至少一种粉体,且所述基体强化粉体粒径为0.01-5μm。Furthermore, the mass fraction of the matrix strengthening powder in the composite powder is 0.05-5%, the matrix strengthening powder includes at least one of Ta powder, Mo powder and W powder, and the particle size of the matrix strengthening powder is 0.01-5 μm.
进一步的,步骤2中,所述TC25G合金粉体名义成分为Further, in step 2, the nominal composition of the TC25G alloy powder is
Ti-6.5Al-4Zr-2Sn-4Mo-1W-0.2Si,且所述TC25G合金球形粉体的粒径为10-300μm。Ti-6.5Al-4Zr-2Sn-4Mo-1W-0.2Si, and the particle size of the TC25G alloy spherical powder is 10-300 μm.
进一步的,通过步骤4所得到的钛基复合材料的基体组织为由α相和β相组成的类网篮状结构;其中α相为片层状,包含微米级初生α相和纳米级次生α相;β相被相互交织的α相分隔开来。所述初生α相片层长度为1-50μm、宽度为0.5-3μm;所述次生α相片层长度为0.05-2μm、宽度为10-200nm。Furthermore, the matrix structure of the titanium-based composite material obtained by step 4 is a basket-like structure composed of α phase and β phase; wherein the α phase is lamellar, including micron-sized primary α phase and nanometer-sized secondary α phase; and the β phase is separated by the interwoven α phase. The primary α phase lamella length is 1-50 μm and the width is 0.5-3 μm; the secondary α phase lamella length is 0.05-2 μm and the width is 10-200 nm.
进一步的,通过步骤4所得到的钛基复合材料,室温下的抗拉强度σb大于1300Mpa、延伸率δ大于7%;700℃下的抗拉强度σb大于650MPa,延伸率δ大于20%Furthermore, the titanium-based composite material obtained by step 4 has a tensile strength σ b greater than 1300 MPa and an elongation δ greater than 7% at room temperature; a tensile strength σ b greater than 650 MPa and an elongation δ greater than 20% at 700°C.
本发明的有益效果是:The beneficial effects of the present invention are:
1、本发明所选基体为TC25G双相钛合金,所述合金具备多重优势,包括耐高温、高强度、高韧性以及可热处理强化等特点。相较于近α型的高温钛合金,TC25G由于其含有较高的β稳定元素,因此在组织调控和性能提升方面具备更大的潜力。所述合金长时间服役的温度可达550℃,为满足高温环境下的应用提供了可靠的性能基础。1. The matrix selected in the present invention is TC25G dual-phase titanium alloy, which has multiple advantages, including high temperature resistance, high strength, high toughness, and heat treatment strengthening. Compared with near-α-type high-temperature titanium alloys, TC25G has greater potential in organizational regulation and performance improvement due to its high content of β-stabilizing elements. The alloy can be used for a long time at a temperature of up to 550°C, providing a reliable performance foundation for applications in high-temperature environments.
2、本发明基于“多效应响应”思想,通过在材料中引入不同尺寸的增强体,并将它们置于材料的不同位置以承担载荷,以实现多层次、多效应的材料响应。具体措施包括引入TiB晶须,有效地限制了原始晶粒的尺寸;引入稀土氧化物Y2O3或La2O3,有效地降低了粉末冶金过程中的氧含量;引入快共析Si元素,有效地强化了基体相界面;引入高熔点的Ta、Mo或W元素,发挥了固溶强化作用,提升了基体的耐热性。这些元素之间通过多元素的耦合作用,共同促进了复合材料强塑性的提升。这一设计理念通过协同作用的多种效应,全面提高复合材料的性能,实现了在不同层次上对材料性能的优化响应。2. The present invention is based on the concept of "multi-effect response". It introduces reinforcements of different sizes into the material and places them at different positions of the material to bear the load, so as to achieve multi-level and multi-effect material response. Specific measures include the introduction of TiB whiskers, which effectively limits the size of the original grains; the introduction of rare earth oxides Y2O3 or La2O3 , which effectively reduces the oxygen content in the powder metallurgy process; the introduction of fast eutectoid Si elements, which effectively strengthens the matrix phase interface; the introduction of high melting point Ta, Mo or W elements, which play a role in solid solution strengthening and improve the heat resistance of the matrix. These elements jointly promote the improvement of the strength and plasticity of the composite material through the coupling effect of multiple elements. This design concept comprehensively improves the performance of the composite material through the synergistic effects of multiple effects, and achieves an optimized response to material properties at different levels.
3、本发明采用的制备方法简单、稳定且可控性强,利用粉末冶金技术实现了对增强相种类和含量的调控。同时,通过引入合金中的高温薄弱区-相界面处的第二相,形成多级、多尺度的增强相分布,提升了界面的高温强度。3. The preparation method adopted by the present invention is simple, stable and highly controllable, and the type and content of the reinforcing phase are regulated by powder metallurgy technology. At the same time, by introducing the second phase at the high-temperature weak zone-phase interface in the alloy, a multi-level and multi-scale reinforcing phase distribution is formed, thereby improving the high-temperature strength of the interface.
4、本发明通过对基体组织的调控,实现了多级多尺度的类网篮状组织,该组织结构在室温和高温条件下表现出卓越的强塑性匹配,实现了材料内部结构的复杂而有序的编织,使其在室温和高温环境下都能够兼顾强度和塑性,同时具备较高的抗断裂和抗蠕变性能,使其符合设计要求中关于室温强塑性匹配和高温抗力的优越性。4. The present invention realizes a multi-level and multi-scale basket-like structure by regulating the matrix organization. This organizational structure shows excellent strength-plasticity matching at room temperature and high temperature conditions, and realizes a complex and orderly weaving of the internal structure of the material, so that it can take into account both strength and plasticity at room temperature and high temperature environments, and at the same time has high fracture resistance and creep resistance, so that it meets the design requirements for room temperature strength-plasticity matching and high temperature resistance.
附图说明BRIEF DESCRIPTION OF THE DRAWINGS
图1是本发明一种兼具高强韧与700℃服役性能的钛基复合材料制备方法的流程图;FIG1 is a flow chart of a method for preparing a titanium-based composite material having both high strength and toughness and 700° C. service performance according to the present invention;
图2是实施例1制备的钛基复合材料扫描电镜图;FIG2 is a scanning electron microscope image of the titanium-based composite material prepared in Example 1;
图3是实施例1制备的钛基复合材料的室温及700℃下的拉伸性能曲线图;FIG3 is a graph showing the tensile properties of the titanium-based composite material prepared in Example 1 at room temperature and 700° C.;
图4是实施例2制备的钛基复合材料扫描电镜图;FIG4 is a scanning electron microscope image of the titanium-based composite material prepared in Example 2;
图5是实施例2制备的钛基复合材料的室温及700℃下的拉伸性能曲线图;FIG5 is a graph showing the tensile properties of the titanium-based composite material prepared in Example 2 at room temperature and 700° C.;
图6是实施例3制备的钛基复合材料扫描电镜图;FIG6 is a scanning electron microscope image of the titanium-based composite material prepared in Example 3;
图7是实施例3制备的钛基复合材料的室温及700℃下的拉伸性能曲线图。FIG. 7 is a graph showing the tensile properties of the titanium-based composite material prepared in Example 3 at room temperature and 700° C.
图8是实施例1至3制备的钛基复合材料的室温及700℃下的拉伸性能曲线比较图。FIG8 is a comparison diagram of the tensile property curves of the titanium-based composite materials prepared in Examples 1 to 3 at room temperature and at 700° C.
具体实施例Specific embodiments
通过下面给出的本发明的具体实施例可以进一步清楚地了解本发明。但它们不是对本发明地限定。The present invention can be further understood by the following specific examples of the present invention, but they are not intended to limit the present invention.
实施例一:Embodiment 1:
如图1所示,本发明的具体实施例中,一种兼具高强韧与700℃服役性能的钛基复合材料制备方法,具体步骤如下:As shown in FIG. 1 , in a specific embodiment of the present invention, a method for preparing a titanium-based composite material having both high strength and toughness and 700° C. service performance comprises the following specific steps:
步骤1、根据设计的增强相或增强元素的含量,计算出的TC25G合金粉体和外加粉体M的质量比如下。外加粉体M按所发挥的作用分类包括原始β晶界强化粉体、α/β相界强化粉体以及基体强化粉体。Step 1. According to the designed content of reinforcing phase or reinforcing element, the calculated mass ratio of TC25G alloy powder and additional powder M is as follows. The additional powder M is classified into original β grain boundary strengthening powder, α/β phase boundary strengthening powder and matrix strengthening powder according to the role played.
其中,原始β晶界强化粉体包括TiB2粉和Y粉(即,钇粉),且所述原始β晶界强化粉体在所述复合粉体中所占质量分数为5%;所述原始β晶界强化粉体粒径为0.05-10μm;The original β grain boundary strengthening powder includes TiB2 powder and Y powder (ie, yttrium powder), and the mass fraction of the original β grain boundary strengthening powder in the composite powder is 5%; the particle size of the original β grain boundary strengthening powder is 0.05-10 μm;
α/β相界强化粉体包括Si粉,且所述α/β相界强化粉体在所述复合粉体中所占质量分数为1%;所述α/β相界强化粉体的粒径为0.05-5μm;The α/β phase boundary strengthening powder includes Si powder, and the mass fraction of the α/β phase boundary strengthening powder in the composite powder is 1%; the particle size of the α/β phase boundary strengthening powder is 0.05-5 μm;
基体强化粉体包括W粉,且所述基体强化粉体在所述复合粉体中所占质量分数为0.05%;所述基体强化粉体粒径为0.01-5μm。The matrix reinforcement powder includes W powder, and the mass fraction of the matrix reinforcement powder in the composite powder is 0.05%; the particle size of the matrix reinforcement powder is 0.01-5 μm.
步骤2、按照设计的质量比称取TC25G合金(也是基体合金)粉体与外加粉体M,进行球磨混合,使粉体混合均匀,获得复合粉体。Step 2: Weigh TC25G alloy (also the matrix alloy) powder and the added powder M according to the designed mass ratio, and mix them by ball milling to make the powders evenly mixed to obtain composite powder.
其中,采用的TC25G钛合金粉体的名义成分为Ti-6.5Al-4Zr-2Sn-4Mo-1W-0.2Si,而且TC25G合金球形粉体粒径为10-300μm。Among them, the nominal composition of the TC25G titanium alloy powder used is Ti-6.5Al-4Zr-2Sn-4Mo-1W-0.2Si, and the particle size of the TC25G alloy spherical powder is 10-300μm.
所述球磨混合中,球磨机的转速为250r/min、持续球磨时间为5h、球料比为4:1、球磨气氛为Ar气。During the ball milling mixing, the rotation speed of the ball mill is 250 r/min, the ball milling time is 5 h, the ball-to-material ratio is 4:1, and the ball milling atmosphere is Ar gas.
步骤3、将获得的所述复合粉体在真空密闭容器中进行热压烧结,并进行原位自生反应制备获得块体复合材料。通过原位自生反应的方式使基体合金的原始β晶粒边界、α/β相界面、基体成分及组织三个层级获得增强。Step 3: hot-pressing and sintering the obtained composite powder in a vacuum-sealed container, and performing an in-situ autogenous reaction to prepare a bulk composite material. The original β grain boundary, α/β phase interface, matrix composition and organization of the matrix alloy are enhanced by the in-situ autogenous reaction.
添加的TiB2粉通过原位自生反应,在原始β晶粒边界处生成TiB晶须。反应生成的TiB晶须呈短棒状或针状,长度为1-50μm、宽度为0.1-5μm。所述TiB晶须,发挥承担载荷的作用,提升材料在室温及高温下的强度。同时TiB作为α相的形核位点,能够显著细化基体晶粒,避免粗大的魏氏体组织出现,提升材料的强度及塑性。The added TiB2 powder generates TiB whiskers at the original β grain boundaries through an in-situ autogenous reaction. The TiB whiskers generated by the reaction are short rod-shaped or needle-shaped, with a length of 1-50 μm and a width of 0.1-5 μm. The TiB whiskers play a role in bearing loads and improve the strength of the material at room temperature and high temperature. At the same time, TiB, as a nucleation site for the α phase, can significantly refine the matrix grains, avoid the appearance of coarse Widmanstatten structure, and improve the strength and plasticity of the material.
添加的Y粉在原始β晶界处与O反应生成稳定的高熔点化合物Y2O3,反应生成的Y2O3为颗粒状,尺寸为0.05-10μm。Y2O3弥散分布在基体合金中,起到弥散强化的作用,有利于提高基体合金的高温瞬时强度和持久强度。此外,基体和界面处的O含量的减少,又解决了粉末冶金脆性的问题,提升了材料塑性。The added Y powder reacts with O at the original β grain boundary to generate a stable high melting point compound Y 2 O 3. The Y 2 O 3 generated by the reaction is in granular form with a size of 0.05-10μm. Y 2 O 3 is dispersed in the matrix alloy, playing a role of dispersion strengthening, which is beneficial to improving the high temperature instantaneous strength and endurance strength of the matrix alloy. In addition, the reduction of O content in the matrix and the interface solves the problem of powder metallurgy brittleness and improves the plasticity of the material.
添加的Si粉通过原位自生反应在α/β相界面处生成(Ti,Zr)5Si3和(Ti,Zr)6Si3中至少一种增强相,并分布在α和β相界面处。反应生成的增强体为亚微米级颗粒状,尺寸为0.01-5μm。弥散析出的硅化物可承担载荷并有效阻碍位错运动,提高钛合金的高温强度和蠕变抗性。The added Si powder generates at least one of the reinforcing phases (Ti,Zr) 5 Si 3 and (Ti,Zr) 6 Si 3 at the α/β phase interface through an in-situ autogenous reaction and is distributed at the α and β phase interfaces. The reinforcement generated by the reaction is in the form of submicron particles with a size of 0.01-5μm. The dispersed silicide can bear the load and effectively hinder the dislocation movement, thereby improving the high temperature strength and creep resistance of the titanium alloy.
基体的强化主要来源于在外加元素W(即强化元素)对材料成分及组织作用。外加元素W在原子尺度上固溶在基体晶体中发挥强韧化效果,进而提升基体钛合金的高温抗软化能力。成分上的作用是指高熔点的W元素固溶在晶格中,一方面发挥固溶强化的效果,另一方面提升材料在高温下的稳定性。组织上的强化是指通过热变形调控出多尺度微观结构的基体。The strengthening of the matrix mainly comes from the effect of the added element W (i.e., strengthening element) on the material composition and organization. The added element W is dissolved in the matrix crystal at the atomic scale to exert a strengthening and toughening effect, thereby improving the high-temperature softening resistance of the matrix titanium alloy. The effect on composition refers to the high-melting-point W element being dissolved in the lattice, which, on the one hand, exerts a solid solution strengthening effect, and on the other hand, improves the stability of the material at high temperatures. Organizational strengthening refers to the control of the matrix with a multi-scale microstructure through thermal deformation.
所述热压烧结中,热压烧结温度为1300℃、热压烧结压力为30MPa、烧结时间为1h。In the hot pressing sintering, the hot pressing sintering temperature is 1300° C., the hot pressing sintering pressure is 30 MPa, and the sintering time is 1 hour.
步骤4、将获得的所述块体复合材料进行热挤压调控基体组织,进一步细化晶粒,获得兼具优异室温强塑性与700℃以上服役性能的钛基复合材料(也是多尺度的基体组织)。Step 4: hot-extrude the obtained bulk composite material to regulate the matrix structure, further refine the grains, and obtain a titanium-based composite material (also a multi-scale matrix structure) with excellent room temperature strength and plasticity and service performance above 700°C.
如图2所示,该基体组织为α相与β相形成类网篮状组织。α相为片层状,包括微米级初生α相和纳米级次生α相,β相被相互交织的α相分隔。所述初生α相片层长度为1-50μm、宽度为0.5-3μm;所述次生α相片层长度为0.05-2μm,宽度为10-200nm。As shown in FIG2 , the matrix structure is a basket-like structure formed by the α phase and the β phase. The α phase is lamellar, including a micron-sized primary α phase and a nanometer-sized secondary α phase, and the β phase is separated by the interwoven α phases. The primary α phase lamellae are 1-50 μm long and 0.5-3 μm wide; the secondary α phase lamellae are 0.05-2 μm long and 10-200 nm wide.
TiB晶须在变形后(即热挤压处理后)的原始基体球界面处沿挤压方向增强相近似线性排布,垂直于挤压方向近似网状分布。Y2O3颗粒分布于变形后(即热挤压处理后)的原始基体球界面处。 TiB whiskers are arranged linearly along the extrusion direction at the interface of the original matrix ball after deformation (i.e. after hot extrusion treatment), and are distributed in a network shape perpendicular to the extrusion direction. Y2O3 particles are distributed at the interface of the original matrix ball after deformation (i.e. after hot extrusion treatment).
进行热挤压时将块体材料在箱式热处理炉中保温30min、保温温度为1000℃、挤压模具保温300℃、挤压比为13:1。During hot extrusion, the block material is kept warm in a box-type heat treatment furnace for 30 minutes, the holding temperature is 1000°C, the extrusion die is kept warm at 300°C, and the extrusion ratio is 13:1.
如图3所示,通过上述步骤所制备的兼具室温强塑性与服役性的钛基复合材料,其室温下抗拉强度σb为1310Mpa、延伸率δ为8.8%;700℃下抗拉强度σb为712MPa,延伸率δ为22%。As shown in FIG3 , the titanium-based composite material having both room temperature strong plasticity and serviceability prepared by the above steps has a room temperature tensile strength σ b of 1310 MPa and an elongation δ of 8.8%; a tensile strength σ b of 712 MPa and an elongation δ of 22% at 700° C.
实施例二:Embodiment 2:
如图1所示,本发明的具体实施例中,一种兼具高强韧与700℃服役性能的钛基复合材料制备方法,具体步骤如下:As shown in FIG. 1 , in a specific embodiment of the present invention, a method for preparing a titanium-based composite material having both high strength and toughness and 700° C. service performance comprises the following specific steps:
步骤1、根据所设计的增强相或增强元素的含量,计算出的TC25G合金粉体和外加粉体M的质量比如下。外加粉体M按所发挥的作用分类包括原始β晶界强化粉体、α/β相界强化粉体以及基体强化粉体。Step 1: According to the content of the designed reinforcing phase or reinforcing element, the calculated mass ratio of the TC25G alloy powder and the additional powder M is as follows. The additional powder M is classified into original β grain boundary strengthening powder, α/β phase boundary strengthening powder and matrix strengthening powder according to the role played.
其中,原始β晶界强化粉体包括TiB2粉和La粉(即镧粉),且所述原始β晶界强化粉体在所述复合粉体中所占质量分数为2.5%;所述原始β晶界强化粉体粒径为0.05-10μm;The original β grain boundary strengthening powder includes TiB2 powder and La powder (i.e. lanthanum powder), and the mass fraction of the original β grain boundary strengthening powder in the composite powder is 2.5%; the particle size of the original β grain boundary strengthening powder is 0.05-10 μm;
α/β相界强化粉体包括Si粉,且所述α/β相界强化粉体在所述复合粉体中所占质量分数为0.05%;所述α/β相界强化粉体的粒径为0.05-5μm;The α/β phase boundary strengthening powder includes Si powder, and the mass fraction of the α/β phase boundary strengthening powder in the composite powder is 0.05%; the particle size of the α/β phase boundary strengthening powder is 0.05-5 μm;
基体强化粉体包括Mo粉,且所述基体强化粉体在所述复合粉体中所占质量分数为5%;所述基体强化粉体粒径为0.01-5μm。The matrix strengthening powder includes Mo powder, and the mass fraction of the matrix strengthening powder in the composite powder is 5%; the particle size of the matrix strengthening powder is 0.01-5 μm.
步骤2、按照设计的质量比称取TC25G合金(也是基体合金)粉体与外加粉体M,进行球磨混合,使粉体混合均匀,获得复合粉体。Step 2: Weigh TC25G alloy (also matrix alloy) powder and external powder M according to the designed mass ratio, and mix them by ball milling to make the powders evenly mixed to obtain composite powder.
其中,采用的TC25G钛合金粉体的名义成分为Ti-6.5Al-4Zr-2Sn-4Mo-1W-0.2Si,而且TC25G合金球形粉体粒径为10-300μm。Among them, the nominal composition of the TC25G titanium alloy powder used is Ti-6.5Al-4Zr-2Sn-4Mo-1W-0.2Si, and the particle size of the TC25G alloy spherical powder is 10-300μm.
所述球磨混合中,球磨机的转速为180r/min、持续球磨时间为5h、球料比为3:1、球磨气氛为Ar气。During the ball milling mixing, the rotation speed of the ball mill is 180 r/min, the ball milling time is 5 h, the ball-to-material ratio is 3:1, and the ball milling atmosphere is Ar gas.
步骤3、将获得的所述复合粉体在真空密闭容器中进行热压烧结,并进行原位自生反应制备获得块体复合材料。通过原位自生反应的方式使基体合金的原始β晶粒边界、α/β相界面、基体成分及组织三个层级获得增强。Step 3: hot-pressing and sintering the obtained composite powder in a vacuum-sealed container, and performing an in-situ autogenous reaction to prepare a bulk composite material. The original β grain boundary, α/β phase interface, matrix composition and organization of the matrix alloy are enhanced by the in-situ autogenous reaction.
添加的TiB2粉通过原位自生反应,在原始β晶粒边界处生成TiB晶须。反应生成的TiB晶须呈短棒状或针状,长度为1-50μm、宽度为0.1-5μm。所述TiB晶须,发挥承担载荷的作用,提升材料在室温及高温下的强度。同时TiB作为α相的形核位点,能够显著细化基体晶粒,避免粗大的魏氏体组织出现,提升材料的强度及塑性。The added TiB2 powder generates TiB whiskers at the original β grain boundaries through an in-situ autogenous reaction. The TiB whiskers generated by the reaction are short rod-shaped or needle-shaped, with a length of 1-50 μm and a width of 0.1-5 μm. The TiB whiskers play a role in bearing loads and improve the strength of the material at room temperature and high temperature. At the same time, TiB, as a nucleation site for the α phase, can significantly refine the matrix grains, avoid the appearance of coarse Widmanstatten structure, and improve the strength and plasticity of the material.
添加的La粉在原始β晶界处与O反应生成稳定的高熔点化合物La2O3,反应生成的La2O3为颗粒状,尺寸为0.05-10μm。La2O3弥散分布在基体合金中,起到弥散强化的作用,有利于提高基体合金的高温瞬时强度和持久强度。此外,基体和界面处的O含量的减少,又解决了粉末冶金脆性的问题,提升了材料塑性。The added La powder reacts with O at the original β grain boundary to generate a stable high melting point compound La 2 O 3. The La 2 O 3 generated by the reaction is in granular form with a size of 0.05-10μm. La 2 O 3 is dispersed in the matrix alloy, playing a role of dispersion strengthening, which is beneficial to improving the high temperature instantaneous strength and endurance strength of the matrix alloy. In addition, the reduction of O content in the matrix and the interface solves the problem of powder metallurgy brittleness and improves the plasticity of the material.
添加的Si粉通过原位自生反应在α/β相界面处生成(Ti,Zr)5Si3和(Ti,Zr)6Si3中至少一种增强相,并分布在α和β相界面处。反应生成的增强体为亚微米级颗粒状,尺寸为0.01-5μm。弥散析出的硅化物可承担载荷并有效阻碍位错运动,提高钛合金的高温强度和蠕变抗性。The added Si powder generates at least one of the reinforcing phases (Ti,Zr) 5 Si 3 and (Ti,Zr) 6 Si 3 at the α/β phase interface through an in-situ autogenous reaction and is distributed at the α and β phase interfaces. The reinforcement generated by the reaction is in the form of submicron particles with a size of 0.01-5μm. The dispersed silicide can bear the load and effectively hinder the dislocation movement, thereby improving the high temperature strength and creep resistance of the titanium alloy.
基体的强化主要来源于在外加元素Mo(即强化元素)对材料成分及组织作用。外加元素Mo在原子尺度上固溶在基体晶体中发挥强韧化效果。进而提升基体钛合金的高温抗软化能力。成分上的作用是指高熔点的Mo元素固溶在晶格中,一方面发挥固溶强化的效果,另一方面提升材料在高温下的稳定性。组织上的强化是指通过热变形调控出多尺度微观结构的基体。The strengthening of the matrix mainly comes from the effect of the added element Mo (i.e. strengthening element) on the material composition and structure. The added element Mo is dissolved in the matrix crystal at the atomic scale to exert a strengthening and toughening effect. This in turn improves the high-temperature softening resistance of the matrix titanium alloy. The effect on the composition refers to the high-melting-point Mo element being dissolved in the lattice, which on the one hand exerts a solid solution strengthening effect, and on the other hand improves the stability of the material at high temperatures. The strengthening of the structure refers to the matrix with a multi-scale microstructure that is regulated by thermal deformation.
所述热压烧结中,热压烧结温度为1200℃、热压烧结压力为30MPa、烧结时间为1h。In the hot pressing sintering, the hot pressing sintering temperature is 1200° C., the hot pressing sintering pressure is 30 MPa, and the sintering time is 1 hour.
步骤4、将获得的所述块体复合材料进行热挤压调控基体组织,进一步细化晶粒,获得兼具优异室温强塑性与700℃以上服役性能的钛基复合材料(也是多尺度的基体组织)。Step 4: hot-extrude the obtained bulk composite material to regulate the matrix structure, further refine the grains, and obtain a titanium-based composite material (also a multi-scale matrix structure) with excellent room temperature strength and plasticity and service performance above 700°C.
如图4所示,该基体组织为α相与β相形成类网篮状组织。α相为片层状,包括微米级初生α相和纳米级次生α相,β相被相互交织的α相分隔。所述初生α相片层长度为1-50μm、宽度为0.5-3μm;所述次生α相片层长度为0.05-2μm,宽度为10-200nm。As shown in FIG4 , the matrix structure is a basket-like structure formed by the α phase and the β phase. The α phase is lamellar, including a micron-sized primary α phase and a nanometer-sized secondary α phase, and the β phase is separated by the interwoven α phases. The primary α phase lamellae are 1-50 μm long and 0.5-3 μm wide; the secondary α phase lamellae are 0.05-2 μm long and 10-200 nm wide.
TiB晶须在变形后(即热挤压处理后)的原始基体球界面处沿挤压方向增强相近似线性排布,垂直于挤压方向近似网状分布。La2O3颗粒分布于变形后(即热挤压处理后)的原始基体球界面处。TiB whiskers are arranged linearly along the extrusion direction at the interface of the original matrix ball after deformation (i.e. after hot extrusion treatment), and are distributed in a network shape perpendicular to the extrusion direction. La 2 O 3 particles are distributed at the interface of the original matrix ball after deformation (i.e. after hot extrusion treatment).
进行热挤压时将块体材料在箱式热处理炉中保温30min、保温温度为1100℃、挤压模具保温400℃、挤压比为13:1。During hot extrusion, the block material is kept warm in a box-type heat treatment furnace for 30 minutes, the holding temperature is 1100°C, the extrusion die is kept warm at 400°C, and the extrusion ratio is 13:1.
如图5所示,通过上述步骤所制备的兼具室温强塑性与服役性的钛基复合材料,室温抗拉强度σb为1402MPa,延伸率δ为10.6%,700℃下抗拉强度σb为720MPa,延伸率δ为27%。As shown in FIG5 , the titanium-based composite material having both room temperature strong plasticity and serviceability prepared by the above steps has a room temperature tensile strength σ b of 1402 MPa and an elongation δ of 10.6%, and a tensile strength σ b of 720 MPa and an elongation δ of 27% at 700°C.
实施例三:Embodiment three:
如图1所示,本发明的具体实施例中,一种兼具高强韧与700℃服役性能的钛基复合材料制备方法,具体步骤如下:As shown in FIG. 1 , in a specific embodiment of the present invention, a method for preparing a titanium-based composite material having both high strength and toughness and 700° C. service performance comprises the following specific steps:
步骤1、根据设计的增强相或增强元素的含量,计算出的TC25G合金粉体和外加粉体M的质量比如下。外加粉体M按所发挥的作用分类包括原始β晶界强化粉体、α/β相界强化粉体以及基体强化粉体。Step 1. According to the designed content of reinforcing phase or reinforcing element, the calculated mass ratio of TC25G alloy powder and additional powder M is as follows. The additional powder M is classified into original β grain boundary strengthening powder, α/β phase boundary strengthening powder and matrix strengthening powder according to the role played.
其中,原始β晶界强化粉体包括B粉(即硼粉)和Y粉,且所述原始β晶界强化粉体在所述复合粉体中所占质量分数为0.05%;所述原始β晶界强化粉体粒径为0.05-10μm;The original β grain boundary strengthening powder includes B powder (i.e., boron powder) and Y powder, and the mass fraction of the original β grain boundary strengthening powder in the composite powder is 0.05%; the particle size of the original β grain boundary strengthening powder is 0.05-10 μm;
α/β相界强化粉体包括Si粉,且所述α/β相界强化粉体在所述复合粉体中所占质量分数为3%;所述α/β相界强化粉体的粒径为0.05-5μm;The α/β phase boundary strengthening powder includes Si powder, and the mass fraction of the α/β phase boundary strengthening powder in the composite powder is 3%; the particle size of the α/β phase boundary strengthening powder is 0.05-5 μm;
基体强化粉体包括Ta粉,且所述基体强化粉体在所述复合粉体中所占质量分数为2%;所述基体强化粉体粒径为0.01-5μm。The matrix strengthening powder includes Ta powder, and the mass fraction of the matrix strengthening powder in the composite powder is 2%; the particle size of the matrix strengthening powder is 0.01-5 μm.
步骤2、按照设计的质量比称取TC25G合金(也是基体合金)粉体与外加粉体M,进行球磨混合,使粉体混合均匀,获得复合粉体。Step 2: Weigh TC25G alloy (also matrix alloy) powder and external powder M according to the designed mass ratio, and mix them by ball milling to make the powders evenly mixed to obtain composite powder.
其中,采用的TC25G钛合金粉体的名义成分为Ti-6.5Al-4Zr-2Sn-4Mo-1W-0.2Si,而且TC25G合金球形粉体粒径为10-300μm。Among them, the nominal composition of the TC25G titanium alloy powder used is Ti-6.5Al-4Zr-2Sn-4Mo-1W-0.2Si, and the particle size of the TC25G alloy spherical powder is 10-300μm.
所述球磨混合中,球磨机的转速为250r/min、持续球磨时间为5h、球料比为4:1、球磨气氛为Ar气。During the ball milling mixing, the rotation speed of the ball mill is 250 r/min, the ball milling time is 5 h, the ball-to-material ratio is 4:1, and the ball milling atmosphere is Ar gas.
步骤3、将获得的所述复合粉体在真空密闭容器中进行热压烧结,并进行原位自生反应制备获得块体复合材料。通过原位自生反应的方式使基体合金的原始β晶粒边界、α/β相界面、基体成分及组织三个层级获得增强。Step 3: hot-pressing and sintering the obtained composite powder in a vacuum-sealed container, and performing an in-situ autogenous reaction to prepare a bulk composite material. The original β grain boundary, α/β phase interface, matrix composition and organization of the matrix alloy are enhanced by the in-situ autogenous reaction.
添加的B粉通过原位自生反应,在原始β晶粒边界处生成TiB晶须。反应生成的TiB晶须呈短棒状或针状,长度为1-50μm、宽度为0.1-5μm。所述TiB晶须,发挥承担载荷的作用,提升材料在室温及高温下的强度。同时TiB作为α相的形核位点,能够显著细化基体晶粒,避免粗大的魏氏体组织出现,提升材料的强度及塑性。The added B powder generates TiB whiskers at the original β grain boundaries through an in-situ autogenous reaction. The TiB whiskers generated by the reaction are short rod-shaped or needle-shaped, with a length of 1-50 μm and a width of 0.1-5 μm. The TiB whiskers play a role in bearing loads and improve the strength of the material at room temperature and high temperature. At the same time, TiB, as a nucleation site for the α phase, can significantly refine the matrix grains, avoid the appearance of coarse Widmanstatten structure, and improve the strength and plasticity of the material.
添加的Y粉在原始β晶界处与O反应生成稳定的高熔点化合物Y2O3,反应生成的Y2O3为颗粒状,尺寸为0.05-10μm。Y2O3弥散分布在基体合金中,起到弥散强化的作用,有利于提高基体合金的高温瞬时强度和持久强度。此外,基体和界面处的O含量的减少,又解决了粉末冶金脆性的问题,提升了材料塑性。The added Y powder reacts with O at the original β grain boundary to generate a stable high melting point compound Y 2 O 3. The Y 2 O 3 generated by the reaction is in granular form with a size of 0.05-10μm. Y 2 O 3 is dispersed in the matrix alloy, playing a role of dispersion strengthening, which is beneficial to improving the high temperature instantaneous strength and endurance strength of the matrix alloy. In addition, the reduction of O content in the matrix and the interface solves the problem of powder metallurgy brittleness and improves the plasticity of the material.
添加的Si粉通过原位自生反应在α/β相界面处生成(Ti,Zr)5Si3和(Ti,Zr)6Si3中至少一种增强相,并分布在α和β相界面处。反应生成的增强体为亚微米级颗粒状,尺寸为0.01-5μm。弥散析出的硅化物可承担载荷并有效阻碍位错运动,提高钛合金的高温强度和蠕变抗性。The added Si powder generates at least one of the reinforcing phases (Ti,Zr) 5 Si 3 and (Ti,Zr) 6 Si 3 at the α/β phase interface through an in-situ autogenous reaction and is distributed at the α and β phase interfaces. The reinforcement generated by the reaction is in the form of submicron particles with a size of 0.01-5μm. The dispersed silicide can bear the load and effectively hinder the dislocation movement, thereby improving the high temperature strength and creep resistance of the titanium alloy.
基体的强化主要来源于在外加元素Ta(即强化元素)对材料成分及组织作用。外加元素Ta在原子尺度上固溶在基体晶体中发挥强韧化效果,进而提升基体钛合金的高温抗软化能力。成分上的作用是指高熔点的Ta元素固溶在晶格中,一方面发挥固溶强化的效果,另一方面提升材料在高温下的稳定性。组织上的强化是指通过热变形调控出多尺度微观结构的基体。The strengthening of the matrix mainly comes from the effect of the added element Ta (i.e., strengthening element) on the material composition and organization. The added element Ta is solid-dissolved in the matrix crystal at the atomic scale to exert a strengthening and toughening effect, thereby improving the high-temperature softening resistance of the matrix titanium alloy. The effect on composition refers to the solid solution of the high-melting-point Ta element in the lattice, which, on the one hand, exerts a solid solution strengthening effect, and on the other hand, improves the stability of the material at high temperatures. Organizational strengthening refers to the control of the matrix with a multi-scale microstructure through thermal deformation.
所述热压烧结中,热压烧结温度为1300℃、热压烧结压力为30MPa、烧结时间为1h。In the hot pressing sintering, the hot pressing sintering temperature is 1300° C., the hot pressing sintering pressure is 30 MPa, and the sintering time is 1 hour.
步骤4、将获得的所述块体复合材料进行热挤压调控基体组织,进一步细化晶粒,获得兼具优异室温强塑性与700℃以上服役性能的钛基复合材料(也是多尺度的基体组织)。Step 4: hot-extrude the obtained bulk composite material to regulate the matrix structure, further refine the grains, and obtain a titanium-based composite material (also a multi-scale matrix structure) with excellent room temperature strength and plasticity and service performance above 700°C.
如图6所示,该基体组织为α相与β相形成类网篮状组织。α相为片层状,包括微米级初生α相和纳米级次生α相,β相被相互交织的α相分隔。所述初生α相片层长度为1-50μm、宽度为0.5-3μm;所述次生α相片层长度为0.05-2μm,宽度为10-200nm。As shown in FIG6 , the matrix structure is a basket-like structure formed by the α phase and the β phase. The α phase is lamellar, including a micron-sized primary α phase and a nanometer-sized secondary α phase, and the β phase is separated by the interwoven α phases. The primary α phase lamellae are 1-50 μm long and 0.5-3 μm wide; the secondary α phase lamellae are 0.05-2 μm long and 10-200 nm wide.
TiB晶须在变形后(即热挤压处理后)的原始基体球界面处沿挤压方向增强相近似线性排布,垂直于挤压方向近似网状分布。Y2O3颗粒分布于变形后(即热挤压处理后)的原始基体球界面处。 TiB whiskers are arranged linearly along the extrusion direction at the interface of the original matrix ball after deformation (i.e. after hot extrusion treatment), and are distributed in a network shape perpendicular to the extrusion direction. Y2O3 particles are distributed at the interface of the original matrix ball after deformation (i.e. after hot extrusion treatment).
进行热挤压时将块体材料在箱式热处理炉中保温30min、保温温度为1000℃、挤压模具保温300℃、挤压比为17:1。During hot extrusion, the block material is kept warm in a box-type heat treatment furnace for 30 minutes, the holding temperature is 1000°C, the extrusion die is kept warm at 300°C, and the extrusion ratio is 17:1.
如图7所示,通过上述步骤所制备的兼具室温强塑性与服役性的钛基复合材料,其室温下抗拉强度σb为1449Mpa、延伸率δ为9.8%;700℃下抗拉强度σb为744MPa,延伸率δ为31%。As shown in FIG7 , the titanium-based composite material with both room temperature ductility and serviceability prepared by the above steps has a room temperature tensile strength σ b of 1449 MPa and an elongation δ of 9.8%; a tensile strength σ b of 744 MPa and an elongation δ of 31% at 700° C.
下面表1中给出了实施例1-3的制备方法中所采用的外加粉体M(如,原始β晶界强化粉体、α/β相界强化粉体以及基体强化粉体)在复合粉体中所占质量分数。Table 1 below shows the mass fraction of the additional powder M (eg, original β grain boundary strengthening powder, α/β phase boundary strengthening powder and matrix strengthening powder) used in the preparation methods of Examples 1-3 in the composite powder.
表1Table 1
下面表2中给出了实施例1-3的制备方法中所采用的外加粉体M(如,原始β晶界强化粉体、α/β相界强化粉体以及基体强化粉体)。The following Table 2 lists the additional powders M (eg, original β grain boundary strengthening powder, α/β phase boundary strengthening powder, and matrix strengthening powder) used in the preparation methods of Examples 1-3.
表2Table 2
下面表3中给出了通过实施例1-3的制备方法所制备出的兼具高强韧与700℃服役性能的钛基复合材在室温和700℃下的性能参数。Table 3 below lists the performance parameters of the titanium-based composite materials having both high strength and toughness and 700° C. service performance prepared by the preparation methods of Examples 1-3 at room temperature and 700° C.
表3table 3
如图8所示,通过三次的实施例结果表明:所述优异综合性能为,室温抗拉强度σb大于1300MPa,延伸率δ大于8%。700℃下抗拉强度σb大于650MPa,延伸率δ大于20%。As shown in FIG8 , the results of three examples show that the excellent comprehensive performance is that the room temperature tensile strength σ b is greater than 1300 MPa, the elongation δ is greater than 8%, the tensile strength σ b is greater than 650 MPa at 700° C., and the elongation δ is greater than 20%.
以上所述,仅是本发明的较佳实施例而已,并非对本发明作任何形式上的限制,虽然本发明已以较佳实施例揭露如上,然而并非用以限定本发明,任何熟悉本专业的技术人员,在不脱离本发明技术方案范围内,当可利用上述揭示的技术内容做出些许更动或修饰为等同变化的等效实施例,但凡是未脱离本发明技术方案内容,依据本发明的技术实质,在本发明的精神和原则之内,对以上实施例所作的任何简单的修改、等同替换与改进等,均仍属于本发明技术方案的保护范围之内。The above description is only a preferred embodiment of the present invention and does not constitute any form of limitation to the present invention. Although the present invention has been disclosed as a preferred embodiment as above, it is not intended to limit the present invention. Any technician familiar with the profession can make some changes or modify the technical contents disclosed above into equivalent embodiments without departing from the scope of the technical solution of the present invention. However, any simple modification, equivalent replacement and improvement of the above embodiments made according to the technical essence of the present invention, within the spirit and principles of the present invention, without departing from the content of the technical solution of the present invention, still fall within the protection scope of the technical solution of the present invention.
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Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1605414A (en) * | 2004-10-22 | 2005-04-13 | 哈尔滨工业大学 | Method for preparing vacuum hotpressing autogeny titanium-base composite material |
CN112195363A (en) * | 2020-08-28 | 2021-01-08 | 中国科学院金属研究所 | High-strength titanium alloy for 500-600 ℃ and processing method thereof |
CN113073232A (en) * | 2021-03-31 | 2021-07-06 | 哈尔滨工业大学 | Ternary micro-nano particle composite reinforced heat-resistant titanium-based composite material and preparation method thereof |
CN115821093A (en) * | 2022-11-25 | 2023-03-21 | 上海交通大学 | Preparation method of multilayer nano-particle reinforced high-strength and high-toughness titanium-based composite material |
CN116005084A (en) * | 2022-12-12 | 2023-04-25 | 华北电力大学 | A kind of W particle-TiB whisker hybrid reinforced titanium matrix composite material and its preparation method |
CN117535608A (en) * | 2023-10-20 | 2024-02-09 | 佛山汇真科技有限公司 | A kind of reinforced phase directional arrangement titanium matrix composite material and its preparation method |
-
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- 2024-02-26 CN CN202410208928.2A patent/CN117966052B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1605414A (en) * | 2004-10-22 | 2005-04-13 | 哈尔滨工业大学 | Method for preparing vacuum hotpressing autogeny titanium-base composite material |
CN112195363A (en) * | 2020-08-28 | 2021-01-08 | 中国科学院金属研究所 | High-strength titanium alloy for 500-600 ℃ and processing method thereof |
CN113073232A (en) * | 2021-03-31 | 2021-07-06 | 哈尔滨工业大学 | Ternary micro-nano particle composite reinforced heat-resistant titanium-based composite material and preparation method thereof |
CN115821093A (en) * | 2022-11-25 | 2023-03-21 | 上海交通大学 | Preparation method of multilayer nano-particle reinforced high-strength and high-toughness titanium-based composite material |
CN116005084A (en) * | 2022-12-12 | 2023-04-25 | 华北电力大学 | A kind of W particle-TiB whisker hybrid reinforced titanium matrix composite material and its preparation method |
CN117535608A (en) * | 2023-10-20 | 2024-02-09 | 佛山汇真科技有限公司 | A kind of reinforced phase directional arrangement titanium matrix composite material and its preparation method |
Non-Patent Citations (1)
Title |
---|
刘静安主编: "《轻合金挤压工模具手册》", vol. 1, 31 January 2012, 冶金工业出版社, pages: 166 - 168 * |
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