CN115821093A - Preparation method of multilayer nano-particle reinforced high-strength and high-toughness titanium-based composite material - Google Patents
Preparation method of multilayer nano-particle reinforced high-strength and high-toughness titanium-based composite material Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
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Abstract
The invention discloses a preparation method of a multilayer nanoparticle reinforced high-toughness titanium-based composite material, which optimizes the organization of a powder metallurgy titanium-based composite material by pre-implanting a superfine net structure nano reinforcement body in powder and prepares the high-toughness nanoparticle reinforced titanium-based composite material, and relates to the field of metal-based composite materials. The method comprises the following steps: (1) Screening titanium-based composite material powder embedded with a superfine net structure; (2) low-temperature pre-pressing and sintering; (3) high-temperature densification sintering; and (4) aging treatment tissue regulation. Finally, the high-toughness titanium-based composite material with uniform and fine microstructure and multi-level distribution of nano reinforcers in crystal boundary/crystal interior is obtained. The method eliminates coarse widmannstatten structures, synchronously refines matrix grains and the sizes of the reinforcements, realizes the fine regulation and control of the sizes and the distribution of the reinforcements, is beneficial to the near-net forming of high-toughness titanium-based composite materials and components thereof, and has important application value in the field of important equipment such as aerospace and the like.
Description
Technical Field
The invention relates to the field of metal matrix composite materials, in particular to a preparation method of a multilayer nanoparticle reinforced high-toughness titanium matrix composite material, which is a strengthening and toughening method of a multilayer nanoparticle reinforced titanium matrix composite material.
Background
The titanium-based composite material has the excellent performances of low density, high specific strength, good corrosion resistance, oxidation resistance and the like, and is gradually one of the most potential candidate structural materials in high-tech fields such as automobiles, aerospace and the like. By introducing for example TiB, tiC, re into the titanium alloy matrix 2 O 3 The ceramic particles with high strength and high modulus are optimized in size and distribution, so that the modulus, the wear resistance and the high-temperature oxidation resistance of the titanium-based composite material can be obviously improved, and the titanium-based composite material is one of effective ways for improving the comprehensive mechanical property and the service temperature of the titanium-based composite material at present.
Powder metallurgy is a net forming method for preparing titanium-based composite materials, compared with other titanium-based composite material preparation technologies based on liquid phase reaction, the method has stronger controllability and designability, the size and distribution of a reinforcement are regulated and controlled by designing a powder structure and a powder spreading process, a core-shell structure, a layered structure, a net structure and the like are constructed, the effect of strengthening and toughening the reinforcement in cooperation with the configuration is fully exerted, the comprehensive performance of the composite materials can be greatly improved, and the method has more applications in the fields of aerospace, industry, medical treatment and the like.
The powder pretreatment modes adopted at home and abroad mainly comprise ball milling, electrostatic adsorption, fluidized bed vapor deposition and the like. Namely, a physical method or a chemical method is utilized to embed or adsorb a reactant of the reinforcement on the surface of the titanium alloy, and then in-situ reaction is induced on the surface of titanium alloy particles in the high-temperature sintering process, so that various reinforcements are generated in the particle boundary. However, when the reinforcement is introduced, sintering above the beta transus point of the material is often required to ensure that the in situ reaction is sufficiently carried out and densification of the material is achieved. The increase of the sintering temperature inevitably promotes the growth of matrix grains, thereby forming Widmannstatten structures containing coarse primary beta grains and reducing the mechanical properties of the material. In order to further improve the performance of the composite material, secondary hot processing ways such as forging, rolling and the like are often required to be supplemented after sintering, so that the material preparation process is greatly prolonged, and the production cost is increased. Therefore, how to adopt a simple and effective method to inhibit the growth of matrix grains at high temperature and realize the regulation and control of the size distribution of matrix tissues and reinforcements so as to improve the comprehensive mechanical properties of sintered materials becomes one of the key directions of attention of researchers.
Disclosure of Invention
The invention aims to provide a preparation method of a multilayer nanoparticle reinforced high-toughness titanium-based composite material, aiming at the problems in the prior art. The method controls the initial size of the reinforcement and the net structure by screening the titanium-based composite material powder with different grain diameters and a superfine net structure, and improves the stability of the nano reinforcement in the low-temperature pre-pressing sintering process. And then, densifying the sintered material in a beta phase region to form a block, and optimally regulating and controlling the matrix tissue type and the size and distribution of the reinforcement body through a process. Finally, controlling the distribution of alloy precipitated phases by aging treatment along with the furnace to obtain the high-toughness titanium-based composite material with uniform and fine tissues and nano reinforcers distributed in a grain boundary/intragranular multi-layer manner; the method solves the problem of coarse titanium alloy structure caused by overhigh sintering temperature, avoids the formation of coarse widmannstatten structure, refines matrix grains and the size of the reinforcement, and realizes the accurate regulation and control of the size distribution of the reinforcement, thereby greatly improving the toughness of the sintered titanium-based composite material. The method and the technology are beneficial to guiding the powder metallurgy method to directly prepare the high-strength and high-toughness titanium-based composite material and the component thereof, and have important application value in the field of important equipment such as aerospace and the like.
The purpose of the invention can be realized by the following scheme:
the invention provides a preparation method of a multilayer nanoparticle reinforced high-toughness titanium-based composite material, which comprises the following steps:
A. screening titanium-based composite material powder embedded with a superfine mesh structure with different particle sizes;
B. heating the screened titanium-based composite material powder to the beta phase transition temperature (T) of the material β ) Pre-pressing and sintering at the temperature of 20-200 ℃;
C. raising the furnace temperature to be above Tbeta by 20-300 ℃ for densification sintering;
D. and cooling to the set aging temperature of the material after sintering, and performing aging treatment to obtain the high-toughness titanium-based composite material with the nano reinforcement in which the nano reinforcement is distributed in a crystal boundary/intragranular multilayer manner in the matrix.
Preferably, the titanium-based composite material powder embedded with the ultrafine mesh structure in the step A comprises titanium base and reinforcements, and the reinforcements are distributed in the titanium base in the ultrafine mesh structure; the matrix comprises pure titanium and titanium alloy, and the reinforcement comprises TiB, tiC and La 2 O 3 、Ti 5 Si 3 、(Ti，Zr) x Si 3 (x = 5-6) one or more of the reinforcements, preferably TiB in combination with other reinforcements. The preparation technology of the powder is patent CN110340371A, and the patent describes the preparation method of the powder in detail.
Preferably, the particle size of the titanium-based composite material powder in the step A is one of 15-53 μm, 53-100 μm, 100-150 μm and 150-225 μm. The volume fraction of the reinforcers in the powder is 1-5%, and the reinforcers are all nano-sized (the diameter or the width is less than 100 nm) and distributed in a superfine network structure. The sizes of the internal reticular structures of the powder with different particle sizes are different, the size of the general reticular structure is reduced along with the increase of the volume fraction of the reinforcement and the reduction of the particle size of the powder, the size of the reticular structure is obviously reduced, the size of a single grid is between 2 and 10 mu m, and the length-diameter ratio and the dispersion degree of the reinforcement in the corresponding sintered material are higher.
Preferably, the pre-pressing sintering manner in step B includes one of hot pressing sintering (HP), hot isostatic pressing sintering (HIP), and Spark Plasma Sintering (SPS). The temperature range of the pre-pressing sintering is as follows: beta transus temperature (T) β ) The following temperature is 20-200 ℃, the prepressing temperature is not more than 900 ℃, and the pressure intensity range is as follows: 50-300 MPa, and the heating rate is as follows: 10-200 ℃/min, the heat preservation time is as follows: 5-60 min.
Preferably, the sintering temperature range of the densification sintering in the step C is as follows: beta transus temperature (T) β ) The temperature is 20-300 ℃, and the pressure intensity range is as follows: 50-300 MPa, and the heating rate is as follows: 10-200 ℃/min, the heat preservation time is as follows: 5-240 min. Wherein the sintering mode comprises the following steps: hot pressing sintering (HP), hot isostatic pressing sintering (HIP) and Spark Plasma Sintering (SPS). Generally, the lower the sintering temperature, the faster the heating rate and the shorter the holding time, the smaller the size of matrix grains and the size of the reinforcement in the material, and the higher the strength of the material. However, the sintering temperature is too low, which results in poor material compactness and obvious holes in the material.
Preferably, the aging treatment mode in the step D is furnace cooling to the aging temperature; the aging temperature is 400-800 ℃, and the aging time is 0.5-8 h. The ageing temperature is controlled according to different materials
Preferably, the high-toughness titanium-based composite material in the step D has uniform and fine equiaxial or near-lamellar tissue, the reinforcement is in a nanometer scale, and the high-toughness titanium-based composite material is distributed in a crystal boundary/intragranular multilayer manner in the matrix. The titanium-based composite material has excellent mechanical property, and the strong plasticity is equivalent to that of a titanium-based composite material forging of the same type. Meanwhile, the sizes and the distribution of the crystal grains and the reinforcement can be regulated and controlled through sintering temperature, heat preservation time and powder granularity, under different processes, the isometric structure scale range is 5-20 mu m, and the reinforcement scale range is 100 nm-2 mu m.
Preferably, the high-strength and high-toughness titanium-based composite material can be subjected to post-treatment by utilizing conventional hot processing technology (such as forging, extrusion, rolling and the like).
In summary, compared with the prior art, the invention has the following beneficial effects:
(1) The invention can obtain the ultrafine net structures with different sizes by screening the titanium-based composite material powder with different grain diameters, and obtains the net structures without sizes by screening the grain diameters of the powder, thereby achieving the purpose of regulating and controlling the sizes of the ultrafine net structures. Firstly, the net structure in the powder breaks through the limitation that the traditional powder mixing process can only introduce the reinforcement at the particle boundary of the powder, simultaneously refines the size of the net structure and the size of the reinforcement, and ensures the distribution uniformity of the nano reinforcement embedded in the composite powder; secondly, the sizes of the net-shaped structure and the reinforcing body are increased along with the increase of the particle size of the powder, and the sizes of the reinforcing body and the net-shaped structure can be directly controlled through powder screening.
(2) In the sintering process, the superfine reticular reinforcement bodies are implanted into the powder in advance, so that the reinforcement bodies only undergo thermal diffusion and growth processes at high temperature, the method is essentially different from the traditional method for introducing the reinforcement bodies through in-situ reaction after mechanical powder mixing, and the problems that the reinforcement bodies are not uniformly distributed and impurities are easily introduced after mechanical powder mixing are solved.
(3) The thermal stability of the nano reinforcement is poor, the thermal stability temperature of the nano reinforcement in the powder is controlled below 900 ℃, the stabilization of the nano reinforcement can be promoted through pre-pressing sintering, and the coarsening of the reinforcement in the high-temperature sintering process is reduced.
(4) The invention is mainly suitable for the sintering process with the temperature above Tbeta, and the superfine reticular structure prefabricated in the powder can play an obvious tissue regulation and control effect only when the sintering temperature is higher than the beta phase transition point of the material, thereby obviously thinning crystal grains and inhibiting the formation of thick Widmannstatten tissues while ensuring that the obtained material has higher density. Meanwhile, the distribution form of the reinforcement in the matrix tissue can be accurately regulated and controlled through the optimization of the sintering process, so that the nano reinforcement is distributed in a crystal boundary/intragranular multilayer manner in the matrix.
(5) The sintered nano-particle reinforced titanium-based composite material prepared by the powder metallurgy method has excellent mechanical property, and the strong plasticity of the sintered nano-particle reinforced titanium-based composite material can be equivalent to that of the similar forged titanium-based composite material without secondary thermal deformation processing;
(6) The invention is suitable for various unit reinforced titanium-based composite materials containing TiB and titanium-based composite materials containing TiB reinforcement and other reinforcement hybrid reinforcement, such as TiB + TiC, tiB + Ti 5 Si 3 、TiB+La 2 O 3 And other TiB + Re x O y And TiB + TiC + Re x O y An iso-hybrid enhancement series;
(7) The invention is suitable for pure titanium or titanium alloy matrixes, including Ti-6Al-4V, IMI834 and the like, and has wide application range;
(8) The invention is suitable for various preparation process systems for realizing powder molding under high temperature and high pressure, such as hot-pressing sintering, hot isostatic pressing sintering, plasma discharge sintering and the like;
(9) The superfine net structure prefabricated in the powder can effectively prevent grains from growing during sintering, has obvious grain refining effect and solves the problem of coarse material structure caused by overhigh sintering temperature. The microstructure of the titanium-based composite material prepared by powder modification shows uniform and fine equiaxial or near-lamellar tissue morphology, and the reinforcers are in nanoscale and are distributed in a crystal boundary/intragranular multilayer manner in the matrix, so that the synergistic strengthening effect of the reinforcers can be fully exerted. Compared with the alloy and other composite materials prepared by the same process, the structure is obviously optimized, and the prepared composite material has no anisotropy, uniform structure and excellent mechanical property.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a 1.2vol.% TiB + La solution prepared by the aerosolization method of example 1 2 O 3 IMI834 heat-resistant titanium-based composite material powder section organizational chart; wherein a is the surface morphology of the powder, and b is the cross-sectional structure characteristic of the powder;
FIG. 2 is the 1.2vol.% TiB + La prepared in example 1 2 O 3 IMI834 titanium-based composite microstructure topography (a) and 2.4vol.% TiB + La prepared in example 2 2 O 3 Zeolite/IMI 834 titanium-based composite material micro-setA texture map (b);
FIG. 3 is the sintered state of 1.2vol.% TiB + La of example 1 2 O 3 A schematic diagram of a nano reinforcement positioned in a grain boundary/crystal in an IMI834 composite material;
FIG. 4 is a graph showing the EBSD structure of the titanium-based composite material (b) obtained in example 2 compared with the base alloy (a) obtained in the same process;
FIG. 5 shows the TiB + La nanoparticles prepared in examples 1 and 2 2 O 3 The tensile property at room temperature of the/IMI 834 titanium-based composite material.
Detailed Description
The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the spirit and scope of the invention. The present invention will be described in detail with reference to the following specific examples:
a strengthening and toughening method of a multilayer nanoparticle reinforced titanium-based composite material comprises the following steps:
A. screening titanium-based composite material powder with different particle sizes and embedded with a superfine mesh structure;
B. filling the screened titanium-based composite material powder with different particle sizes into a mould, heating the mould in a sintering furnace along with the furnace to 20-200 ℃ below the beta phase transition temperature of the material, and performing pre-pressing sintering;
C. increasing the furnace temperature to T β Carrying out densification sintering at the temperature of between 20 and 300 ℃;
D. and cooling the sintered material in a furnace to the set aging temperature of the material, and performing aging treatment. And obtaining the high-strength and high-toughness titanium-based composite material with the nano reinforcement body in a matrix in which grain boundaries/intragranular multi-layer distribution is realized.
The titanium-based composite material powder is prepared by the following method:
with TiB + La 2 O 3 Example of composite powder of IMI834
Taking titanium sponge, zirconium sponge, aluminum wire, aluminum molybdenum (Al-Mo), titanium tin (Ti-Sn), aluminum niobium (Al-Nb) and other intermediate alloys as alloy raw materials and hexaborideLanthanum (LaB) 6 ) The powder is taken as a raw material of the reinforcement, and is weighed according to 2.5kg per part, wherein the volume fractions of the reinforcement are controlled to be 1.2vol.% and 2.4vol.%, respectively, and the raw material is poured into a mould and mechanically pressed into a consumable electrode;
step two, putting the electrode into a vacuum consumable arc furnace for first vacuum melting, controlling the melting current to be 1kA and the vacuum degree to be 5 multiplied by 10 -3 Pa, repeating the smelting process for three times to ensure that the components of the ingot are uniform, and completely carrying out in-situ reaction to obtain a third ingot;
step three, forging and drawing the obtained tertiary ingot at 1100 ℃ to obtain a rough blank bar material with the outer diameter of 55mm and the length of 450mm, and machining and polishing the rough blank bar material into a regular round bar with the outer diameter of 50mm and the length of 500mm;
fourthly, adopting electrode induction smelting gas atomization powder making equipment, heating a bar electrode to 2000 ℃ by using an induction coil, enabling the melt to freely flow downwards into a gas atomization furnace through a leakage hole, enabling the atomization pressure to be 2.5MPa, adopting argon gas as gas, crushing the alloy melt into fine liquid drops, quickly cooling to obtain titanium-based composite material powder, and collecting the powder;
and step five, screening the prepared titanium-based composite material powder, and performing particle size distribution according to three particle size distributions of 0-53 microns, 53-150 microns and more than 150 microns to obtain 32% of 15-53 microns powder, 41% of 53-100 microns powder, 22% of 100-150 microns powder and 5% of more than 150 microns powder.
Evaluation criteria and methods:
1. powder texture morphology- -internal TiB, tiC, la 2 O 3 When the reinforcement bodies are distributed in a network structure, the embedding of the reinforcement bodies is realized; the sintered composite material tissue-the material tissue is obviously thinned after the powder modification, and presents a uniform equiaxial tissue, and meanwhile, the reinforcement is uniformly distributed in the matrix in a micro-nano dual-scale manner;
the test method comprises the following steps: the microstructure was observed by applying a voltage of 5kV to TASCAN RISE-MAGNA.
2. Tensile property test- -tensile strength, elongation;
the test method comprises the following steps: the mechanical property test is carried out on a Zwick Z100 universal tester, the sample is a sheet tensile sample, and the elongation is measured by adopting an extensometer.
Example 1
The embodiment provides a strengthening and toughening method of a multilayer nanoparticle reinforced titanium-based composite material, which comprises the following steps:
A. 0.91vol.% TiB +0.29vol.% La prepared by gas atomization method 2 O 3 Reinforced IMI834 composite powder (1.2 vol.% TiB + La) 2 O 3 IMI 834) by vibration screening to obtain powder with particle size of 53-100 μm;
B. filling the screened titanium-based composite material powder with different grain diameters into a mould, and carrying out pre-pressing sintering in a hot-pressing sintering furnace. The temperature range of the pre-pressing sintering is as follows: 900 ℃, pressure range is: 50MPa, and the heating rate is as follows: 10 ℃/min, the heat preservation time is as follows: 60min, vacuum degree greater than 5 × 10 -2 Pa。
C. After the pre-pressing sintering is finished, the temperature is raised to 1200 ℃ along with the furnace for densification sintering, and the sintering pressure is as follows: 50MPa, and the heating rate is as follows: 10 ℃/min, the heat preservation time is as follows: 60min, vacuum degree greater than 5 × 10 -2 Pa。
D. And cooling the sintered material in a furnace to 700 ℃ for aging treatment, and cooling the sintered material in the furnace to room temperature after heat preservation for 2 hours. And obtaining the high-strength and high-toughness titanium-based composite material which has uniform and fine tissues and is provided with the nano reinforcement in a matrix in a way of multi-level distribution of crystal boundary/crystal interior.
FIG. 1 shows the morphology of the powder structure, showing TiB and La inside 2 O 3 The reinforcement bodies are distributed in a network structure, and embedding of the reinforcement bodies is realized. Fig. 2 (a) is a schematic diagram of a sintered structure, coarse primary beta crystals and widmannstatten structures are not observed from the material structure, and the material presents a uniform and fine near-lamellar structure. FIG. 3 is the resulting 1.2vol.% TiB + La 2 O 3 The shape and distribution of the heat-resistant titanium-based composite material reinforcing body of/IMI 834 are schematic, and TiB and La can be seen 2 O 3 All keep nano-size and are distributed in multiple layers in the crystal boundary/crystal inner range. FIG. 5 shows the results of tensile property tests, wherein the tensile strength of 1.2vol.% of the composite material reached 1100MPa, and the elongation of 10% or more was maintained, compared with the base material prepared by the same processCompared with the bulk alloy, the elongation is improved by 5 times on the premise of not losing the strength.
Example 2
The embodiment provides a strengthening and toughening method of a multilayer nanoparticle reinforced titanium-based composite material, which comprises the following steps:
A. 2.4vol TiB + La prepared by gas atomization method 2 O 3 IMI834, screening out powder with particle size of 53-100 μm by vibration screening;
B. filling the screened titanium-based composite material powder with different grain diameters into a mould, and carrying out pre-pressing sintering in a hot-pressing sintering furnace. The temperature range of the pre-pressing sintering is as follows: 900 ℃, pressure range is: 50MPa, and the heating rate is as follows: 10 ℃/min, the heat preservation time is as follows: 60min, vacuum degree greater than 5 × 10 -2 Pa。
C. After the pre-pressing sintering is finished, the temperature is raised to 1100 ℃ along with the furnace for densification sintering, and the sintering pressure is as follows: 50MPa, and the heating rate is as follows: 10 ℃/min, the heat preservation time is as follows: 60min, vacuum degree greater than 5 × 10 -2 Pa。
D. And cooling the sintered material in a furnace to 700 ℃ for aging treatment, and cooling the sintered material in the furnace to room temperature after heat preservation for 2 hours. And obtaining the high-strength and high-toughness titanium-based composite material which has uniform and fine tissues and is provided with the nano reinforcement in a matrix in a way of multi-level distribution of crystal boundary/crystal interior.
In the material prepared in this example, the microstructure morphology is similar to that in example 1, and a network structure is formed in the powder, and in addition, as can be seen from the structure photograph in fig. 2 (b), the increase of the volume fraction of the reinforcement promotes the refinement of the matrix, so that the matrix is further refined into a fine isometric structure, and the purpose of tissue regulation is achieved. FIG. 4 is the resulting 2.4vol.% TiB + La 2 O 3 The EBSD structure comparison graph of the IMI834 heat-resistant titanium-based composite material and the IMI834 matrix alloy in the same process shows that the ultrafine net structure in the composite material powder plays a role in refining grains and regulating and controlling the matrix structure. FIG. 5 is a tensile Property test of 2.4vol.% TiB + La 2 O 3 The tensile strength of the reinforced composite material reaches more than 1181MPa, the elongation is higher than 3.5%, and compared with the matrix alloy prepared by the same process, the strength of the reinforced composite material is higher than that of the matrix alloy prepared by the same processAnd the plasticity is improved simultaneously.
Example 3
The embodiment provides a strengthening and toughening method of a multilayer nanoparticle reinforced titanium-based composite material, which comprises the following steps:
A. 2.5vol.% of TiB/IMI834 prepared by an air atomization method is selected, and powder with the particle size of 15-53 mu m is screened out through vibration screening;
B. filling the screened titanium-based composite material powder with different particle sizes into a mould, and carrying out pre-pressing sintering in a hot-pressing sintering furnace. The prepressing sintering temperature range is as follows: 900 ℃, pressure range is: 50MPa, and the heating rate is as follows: 10 ℃/min, the heat preservation time is as follows: 60min, vacuum degree greater than 5 × 10 -2 Pa。
C. After the pre-pressing sintering is finished, the temperature is raised to 1200 ℃ along with the furnace for densification sintering, and the sintering pressure is as follows: 50MPa, and the heating rate is as follows: 10 ℃/min, the heat preservation time is as follows: 60min, vacuum degree greater than 5 × 10 -2 Pa。
D. And cooling the sintered material in a furnace to 700 ℃ for aging treatment, and cooling the sintered material in the furnace to room temperature after heat preservation for 2 hours. And obtaining the high-strength and high-toughness titanium-based composite material which has uniform and fine tissues and is provided with the nano reinforcement in a matrix in a way of multi-level distribution of crystal boundary/crystal interior.
In the material prepared in this example, the microstructure morphology is similar to that of example 2, a mesh structure is formed in the powder, and the sintered titanium alloy presents a uniform and fine equiaxial structure.
Example 4
The embodiment provides a strengthening and toughening method of a multilayer nanoparticle reinforced titanium-based composite material, which comprises the following steps:
A. selecting 4vol.% of TiB and 1vol.% of TiC enhanced TC4 composite material powder prepared by an atomization method, and screening out powder with the particle size of 53-100 mu m by vibration screening;
B. filling the screened titanium-based composite material powder with different grain diameters into a mould, and carrying out pre-pressing sintering in a hot-pressing sintering furnace. The temperature range of the pre-pressing sintering is as follows: 800 ℃, pressure range is: 50MPa, and the heating rate is as follows: 10 ℃/min, the heat preservation time is as follows: 60min, vacuumDegree greater than 5 x 10 -2 Pa。
C. After the pre-pressing sintering is finished, the temperature is raised to 1200 ℃ along with the furnace for densification sintering, and the sintering pressure is as follows: 50MPa, and the heating rate is as follows: 10 ℃/min, the heat preservation time is as follows: 60min, vacuum degree greater than 5 × 10 -2 Pa。
D. And cooling the sintered material in a furnace to 600 ℃ for aging treatment, and cooling the sintered material in the furnace to room temperature after heat preservation for 2 hours. And obtaining the high-toughness titanium-based composite material which has uniform and fine tissues and is formed by the TiB and TiC nano reinforcement bodies which are distributed in a crystal boundary/intragranular multilayer manner in a matrix.
In the material prepared in this example, the microstructure morphology of the matrix was the same as that of example 2, and all of the microstructure morphology was fine equiaxed. But with the addition of TiC, the sintered structure is further refined, and TiB and TiC nano reinforcement bodies are distributed in a multilayer way in the grain boundary/crystal.
Example 5
The embodiment provides a strengthening and toughening method of a multilayer nanoparticle reinforced titanium-based composite material, which comprises the following steps:
A. selecting 2.5vol.% of TiB and 2.5vol.% of TiC enhanced TC4 composite material powder prepared by an atomization method, and screening the powder with the particle size of 15-53 mu m by vibration screening;
B. filling the screened titanium-based composite material powder with different grain diameters into a mould, and carrying out pre-pressing sintering in a hot-pressing sintering furnace. The temperature range of the pre-pressing sintering is as follows: 800 ℃, pressure range is: 50MPa, and the heating rate is as follows: 10 ℃/min, the heat preservation time is as follows: 60min, vacuum degree greater than 5 × 10 -2 Pa。
C. After the pre-pressing sintering is finished, the temperature is raised to 1200 ℃ along with the furnace for densification sintering, and the sintering pressure is as follows: 50MPa, and the heating rate is as follows: 10 ℃/min, the heat preservation time is as follows: 60min, vacuum degree greater than 5 × 10 -2 Pa。
D. And cooling the sintered material in a furnace to 600 ℃ for aging treatment, and cooling the sintered material in the furnace to room temperature after heat preservation for 2 hours. And obtaining the high-strength and high-toughness titanium-based composite material which has uniform and fine tissues and is provided with TiB and TiC nano reinforcement bodies which are distributed in a crystal boundary/intragranular multilayer manner in a matrix.
In the material prepared by the embodiment, the microstructure morphology of the sintered material is similar to that of the material prepared by the embodiment 2, and the method is proved to be suitable for different titanium alloy systems and composite materials with high volume fractions.
Comparative example 1
The comparative example provides a strengthening and toughening method of a multilayer nanoparticle reinforced titanium-based composite material, which basically comprises the following steps of: the pre-pressing sintering is not carried out, the densification sintering is carried out at 1100-1200 ℃, and the sintering pressure is as follows: 50MPa, and the heating rate is as follows: 10 ℃/min, the heat preservation time is as follows: 120min, vacuum degree greater than 5 × 10 -2 Pa。
Compared with the two-step sintering process, the one-step sintering process can obtain the densified bulk material, but because the nano reinforcement has poor thermal stability at high temperature, the size coarsening of the material reinforcement which is not subjected to low-temperature stabilization treatment is obvious, and the material reinforcement mostly grows into a reinforcement with a micron size, the material strength and plasticity are reduced at the same time, and compared with the material sintered by two steps, the material sintered by one-step densification has the strength reduced by 30-50 MPa, and the elongation is reduced by 1-3%.
Comparative example 2
The comparative example provides a strengthening and toughening method of a multilayer nanoparticle reinforced titanium-based composite material, which basically comprises the following steps of: in step A, conventional equivalent TiB is adopted 2 、La 2 O 3 And C, mixing the reinforcing body reactant with the spherical titanium alloy powder, and performing high-temperature in-situ reaction in the step C to obtain the titanium-based composite material.
The process is similar to the method disclosed in patent CN101333607, and the essential difference is that: (1) The titanium-based composite material powder adopted by the method realizes the homogenization and compounding of the reinforcement before sintering, and does not need homogenization such as ball milling or surface coating processes, so that the preparation flow is shortened, and the introduction of impurities is avoided; (2) The contrast process needs to introduce the reinforcement by utilizing the in-situ reaction of a reactant at high temperature and a matrix, the temperature required by general sintering densification is higher, so that the reinforcement and the matrix are obviously coarsened, the size of the reinforcement is more than 5 mu m, and the matrix is in a thick lamellar structure; (3) The reaction agent of the reinforcement body in the comparative process is generally attached to the surface of the spherical titanium alloy powder, and a reticular structure with the diameter of about 50-150 mu m is formed at the grain boundary after sintering, while the nano reinforcement body of the material obtained by the invention is distributed in multiple layers in the grain boundary/crystal, has higher dispersion degree and has obvious difference in tissue characteristics.
Comparative example 3
The comparative example provides a strengthening and toughening method of a multilayer nanoparticle reinforced titanium-based composite material, which basically comprises the following steps of: and the densification sintering temperature in the step C is 950 ℃ and 1000 ℃ respectively, and is lower than the beta phase transition temperature. Although the grain size can be obviously refined at a low sintering temperature, the compactness of the material is only 91.6% and 96.3% which are far lower than 99.3% of that of the embodiment 1 respectively, a large number of micropores exist in the microstructure of the material, so that the material shows obvious room-temperature brittleness, and the elongation is respectively 1.1% and 4.3% which are far lower than that of the embodiment 1, therefore, the preferable preparation parameters are important basis for regulating and controlling the structure of the material and improving the comprehensive performance.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. A preparation method of a multilayer nanoparticle reinforced high-toughness titanium-based composite material is characterized by comprising the following steps:
A. screening titanium-based composite material powder embedded with a superfine mesh structure with different particle sizes;
B. heating the screened titanium-based composite material powder to 20-200 ℃ below the beta phase transition temperature of the material, and performing pre-pressing sintering;
C. raising the furnace temperature to 20-300 ℃ above the beta phase transition temperature for densification sintering;
D. and cooling to the set aging temperature of the material after sintering, and performing aging treatment to obtain the high-toughness titanium-based composite material with the nano reinforcement in which the nano reinforcement is distributed in a crystal boundary/intragranular multilayer manner in the matrix.
2. The method according to claim 1, wherein in step A, the titanium-based composite powder embedded with the ultrafine mesh structure comprises titanium-based materials and reinforcing bodies, and the reinforcing bodies are distributed in the ultrafine mesh structure in the titanium-based materials.
3. The method of claim 2, wherein the matrix comprises pure titanium and titanium alloy, and the reinforcement comprises TiB, tiC, la 2 O 3 、Ti 5 Si 3 、(Ti，Zr) x Si 3 One or more of the reinforcement bodies, wherein x is 5-6.
4. The preparation method of claim 2, wherein the volume fraction of the reinforcement in the powder is 1-5%, and the reinforcement is nano-sized, has a diameter or width less than 100nm, and is distributed in a superfine network structure.
5. The preparation method according to claim 1, wherein in the step a, the particle size of the titanium-based composite material powder is in one of the ranges of 15 to 53 μm, 53 to 100 μm, 100 to 150 μm, and 150 to 225 μm.
6. The method of claim 1, wherein the pre-press sintering in step B comprises one of hot press sintering, hot isostatic pressing sintering, and spark plasma sintering.
7. The preparation method according to claim 1, wherein in the step B, the pre-pressing sintering temperature is 20-200 ℃ below the beta phase transition temperature, the pressure is 50-300 MPa, the temperature rising rate is 10-200 ℃/min, and the holding time is 5-60 min.
8. The method according to claim 1, wherein the vacuum sintering in step C comprises: hot pressing sintering, hot isostatic pressing sintering and spark plasma sintering.
9. The preparation method according to claim 1, wherein the sintering temperature of the densification sintering in the step C is 20-300 ℃ above the beta transformation temperature, the pressure is 50-300 MPa, the heating rate is 10-200 ℃/min, and the holding time is 5-240 min.
10. The method according to claim 1, wherein the aging treatment in step D is furnace cooling to an aging temperature; the aging temperature is 400-800 ℃, and the aging time is 0.5-8 h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104263984A (en) * | 2014-10-14 | 2015-01-07 | 哈尔滨工业大学（威海） | Preparation method of TiBw/Ti-6Al-4V composite bar adopting quasi-continuous reticular structure |
| CN107385250A (en) * | 2017-07-18 | 2017-11-24 | 湘潭大学 | A kind of preparation method of TiC enhancings Ultra-fine Grained β titanium niobium based composites |
| CN110340371A (en) * | 2019-08-06 | 2019-10-18 | 上海交通大学 | A kind of preparation method of granule intensified titanium-base compound material increasing material manufacturing powder |
| CN111151746A (en) * | 2019-12-31 | 2020-05-15 | 上海交通大学 | Additive manufacturing method of titanium-based composite material of self-generated superfine net structure reinforcement |
-
2022
- 2022-11-25 CN CN202211489986.4A patent/CN115821093A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104263984A (en) * | 2014-10-14 | 2015-01-07 | 哈尔滨工业大学（威海） | Preparation method of TiBw/Ti-6Al-4V composite bar adopting quasi-continuous reticular structure |
| CN107385250A (en) * | 2017-07-18 | 2017-11-24 | 湘潭大学 | A kind of preparation method of TiC enhancings Ultra-fine Grained β titanium niobium based composites |
| CN110340371A (en) * | 2019-08-06 | 2019-10-18 | 上海交通大学 | A kind of preparation method of granule intensified titanium-base compound material increasing material manufacturing powder |
| CN111151746A (en) * | 2019-12-31 | 2020-05-15 | 上海交通大学 | Additive manufacturing method of titanium-based composite material of self-generated superfine net structure reinforcement |
Non-Patent Citations (3)
| Title |
|---|
| SHAOPENG LI、XIAOYAN WANG等: "Simultaneously improving the strength and ductility of the as-sintered (TiB+La2O3)/Ti composites by in-situ planting ultra-fine networks into the composite powder", SCRIPTA MATERIALIA, vol. 218, pages 1 - 7 * |
| SHAOPENG LI、XIAOYAN WANG等: "Towards high strengthening efficiency by in-situ planting nano-TiB networks into titanium matrix composites", COMPOSITES PART B, vol. 245, 4 August 2022 (2022-08-04), pages 1 - 13 * |
| SHAOPENG LI、XIAOYAN WANG等: "Towards high strengthening efficiency by in-situ planting nano-TiB networks into titanium matrix composites", COMPOSITES PART B, vol. 245, pages 1 - 13 * |
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