CN113634989A - Zr-Ta nanosheet reinforced Ti-Mo-based composite material and preparation method thereof - Google Patents

Zr-Ta nanosheet reinforced Ti-Mo-based composite material and preparation method thereof Download PDF

Info

Publication number
CN113634989A
CN113634989A CN202110533591.9A CN202110533591A CN113634989A CN 113634989 A CN113634989 A CN 113634989A CN 202110533591 A CN202110533591 A CN 202110533591A CN 113634989 A CN113634989 A CN 113634989A
Authority
CN
China
Prior art keywords
plate
plates
sheath
composite material
reinforced
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202110533591.9A
Other languages
Chinese (zh)
Other versions
CN113634989B (en
Inventor
郭顺
黄豪
张慧慧
丁旺
沈宝国
刘海霞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jiangsu University
Original Assignee
Jiangsu University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jiangsu University filed Critical Jiangsu University
Priority to CN202110533591.9A priority Critical patent/CN113634989B/en
Publication of CN113634989A publication Critical patent/CN113634989A/en
Application granted granted Critical
Publication of CN113634989B publication Critical patent/CN113634989B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23P—METAL-WORKING NOT OTHERWISE PROVIDED FOR; COMBINED OPERATIONS; UNIVERSAL MACHINE TOOLS
    • B23P15/00—Making specific metal objects by operations not covered by a single other subclass or a group in this subclass
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C16/00—Alloys based on zirconium
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing 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
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/183—High-melting or refractory metals or alloys based thereon of titanium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16—Changing 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
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • C22F1/186—High-melting or refractory metals or alloys based thereon of zirconium or alloys based thereon

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Powder Metallurgy (AREA)

Abstract

The Zr-Ta/Ti-Mo composite material prepared by the method has high yield strength, high tensile strength and large elongation on the premise of keeping a single Body Centered Cubic (BCC) structure, realizes good matching of high strength (including high yield strength and high tensile strength) and large elongation in the BCC structure, can effectively solve the problem of insufficient matching of strength and elongation (expressed as relatively low tensile strength and elongation product) of the existing beta-type titanium alloy when the existing beta-type titanium alloy presents a single BCC structure, and is expected to obtain important application in the high-technology fields of biomedicine, advanced industry and the like.

Description

Zr-Ta nanosheet reinforced Ti-Mo-based composite material and preparation method thereof
Technical Field
The invention relates to a Zr-Ta nanosheet reinforced Ti-Mo based (abbreviated as Zr-Ta/Ti-Mo) composite material and a preparation method thereof.
Background
Titanium alloys have been widely used in the fields of aviation, aerospace, ships, chemical engineering, medical instruments and the like by virtue of their excellent comprehensive mechanical properties (high specific strength), good functional characteristics (shape memory and superelasticity), and excellent biocompatibility and corrosion resistance, and are known as "triphibian metals in sea, land and air". The achievement of the above excellent characteristics of the titanium alloy is mainly benefited by the fact that the titanium alloy can obtain different microscopic phases with different crystal structures through adjusting alloy components and a thermo-mechanical treatment process, wherein the microscopic phases comprise a beta phase with a body-centered cubic structure, an alpha and alpha 'phase with a close-packed hexagonal structure, an alpha' phase with an orthogonal structure and omega with a non-close-packed hexagonal structure. Among the numerous microscopic phases of titanium alloys, the β phase having a Body Centered Cubic (BCC) structure has received attention in the scientific and engineering fields due to its unique properties of low elastic modulus, excellent biocompatibility and greater elongation. At present, biomedical titanium alloys and super-elastic titanium alloys are designed and optimized in performance based on BCC (i.e., beta phase) structures.
Although the beta-phase titanium alloy with the BCC structure has the performance advantages of low elastic modulus, large elongation and the like, the beta-phase titanium alloy also has the performance defects of lower yield strength and tensile strength. In order to improve the yield strength and tensile strength of the BCC titanium alloy, the strengthening is mainly achieved by precipitating an α strengthening phase with a hexagonal close-packed structure or an ω strengthening phase with a hexagonal close-packed structure on a BCC matrix of the titanium alloy by means of thermal-mechanical treatment. However, these strengthening methods inevitably introduce α -phase or ω -phase which is not BCC structure, and destroy the original single BCC structure of β -phase titanium alloy, resulting in the deterioration or even disappearance of some properties of BCC alloy. For example, the introduction of alpha or omega precipitates other than BCC structures into the BCC matrix of a titanium alloy, while increasing the alloy yield and tensile strength, also results in a significant increase in the elastic modulus of the alloy with a concomitant significant decrease in elongation. Research shows that when the content of the omega phase in the titanium alloy exceeds 30% by volume, the titanium alloy does not have the characteristic of low elastic modulus, and the tensile elongation of the titanium alloy is reduced to 3%, which is about 1/7% of BCC titanium alloy. Therefore, on the premise of keeping a single BCC structure, the strength (including yield strength and tensile strength) and elongation of the existing beta-phase titanium alloy are difficult to achieve high matching (the product of tensile strength and elongation is relatively low), and the application of the existing beta-phase titanium alloy in high-tech fields such as biomedicine, advanced industry and the like is limited.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a Zr-Ta nanosheet reinforced Ti-Mo based (abbreviated as Zr-Ta/Ti-Mo) composite material and a preparation method thereof. The invention realizes good matching of high strength (including high yield strength and high tensile strength) and large elongation in the BCC structure by fully exerting the high yield strength and high tensile strength of the Zr-Ta nanoscale reinforcing phase and the excellent elongation of the Ti-Mo matrix and by means of the performance improvement effect given by microstructure factors such as component interface, orientation deviation and the like when two BCC components are compounded, and is expected to obtain important application in the high-technology fields of biomedicine, advanced industry and the like.
The invention belongs to the field of metal matrix composite materials, and relates to a Zr-Ta nanosheet reinforced Ti-Mo based (abbreviated as Zr-Ta/Ti-Mo) composite material and a preparation method thereof.
Drawings
FIG. 1 shows a schematic view of a stack of Ti-Mo and Zr-Ta plates in a production process according to an embodiment of the present invention.
FIG. 2 is a schematic illustration of a hot extruded and split rolled can for use in a method of making according to one embodiment of the present invention.
FIG. 3 shows Zr prepared according to example 1 of the present invention70Ta30Nanosheet reinforced Ti90Mo10High energy X-ray diffraction patterns of the base composite.
FIG. 4 shows Zr prepared according to example 1 of the present invention70Ta30Nanosheet reinforced Ti90Mo10Scanning electron microscope photograph of the cross section of the base composite material.
FIG. 5 shows Zr prepared according to example 1 of the present invention70Ta30Nanosheet reinforced Ti90Mo10Stress-strain curves of the base composite during stretching.
FIG. 6 shows Zr prepared according to example 2 of the present invention60Ta40Nanosheet reinforced Ti85Mo15High energy X-ray diffraction patterns of the base composite.
FIG. 7 shows Zr prepared according to example 2 of the present invention60Ta40Nanosheet reinforced Ti85Mo15Scanning electron microscope photograph of the cross section of the base composite material.
FIG. 8 shows Zr prepared according to example 2 of the present invention60Ta40Nanosheet reinforced Ti85Mo15Stress-strain curves of the base composite during stretching.
FIG. 9 shows Zr prepared according to example 3 of the present invention50Ta50Nanosheet reinforced Ti80Mo20High energy X-ray diffraction patterns of the base composite.
FIG. 10 shows Zr prepared according to example 3 of the present invention50Ta50Nanosheet reinforced Ti80Mo20Scanning electron microscope photograph of the cross section of the base composite material.
FIG. 11 shows Zr prepared according to example 3 of the present invention50Ta50Nanosheet reinforced Ti80Mo20Stress-strain curves of the base composite during stretching.
Detailed Description
According to the invention, in order to solve the problem that the strength (including yield strength and tensile strength) and elongation of the existing titanium alloy are difficult to realize higher matching when a single BCC structure is maintained, the invention provides a Zr-Ta nanosheet reinforced Ti-Mo-based (abbreviated as Zr-Ta/Ti-Mo) composite material and a preparation method thereof. The invention realizes good matching of high strength (including high yield strength and high tensile strength) and large elongation in the BCC structure by fully exerting the high yield strength and high tensile strength of the Zr-Ta nanoscale reinforcing phase and the excellent elongation of the Ti-Mo matrix and by means of the performance improvement effect given by microstructure factors such as component interface, orientation deviation and the like when two BCC components are compounded, and can be expected to meet the urgent requirements of high-technical fields such as biomedicine, advanced industry and the like on the titanium-based composite material with high tensile strength and elongation product.
According to one aspect of the present invention, the Zr-Ta/Ti-Mo composite material according to the present invention is prepared by using the following raw material types:
reinforcing materials: Zr-Ta alloy (wherein the mass percentage of Ta is 30-50%, and the balance is Zr);
base material: the alloy is Ti-Mo alloy (wherein the mass percentage of Mo is 10-20%, and the balance is Ti).
The raw materials can be prepared according to the component proportion, and can also be purchased in batches at home, namely, the raw materials required by the invention do not need to be imported. The Zr-Ta alloy and the Ti-Mo matrix alloy for reinforcement are alternately arranged to form a layered composite structure according to the mode shown in figure 1, wherein the thickness of the Zr-Ta alloy in the composite material accounts for 15-25%, and the balance is the Ti-Mo matrix alloy.
According to a further aspect of the present invention, there is provided a process for preparing a Zr-Ta/Ti-Mo composite material according to the present invention, comprising the steps of:
firstly, respectively cutting Zr-Ta and Ti-Mo raw material plates from a Zr-Ta alloy and a Ti-Mo alloy by adopting a linear cutting and/or machining method, and obtaining the Zr-Ta and Ti-Mo plates with fresh surfaces (without dirt or surface oxide scales) by mechanically grinding and ultrasonically cleaning the two raw material plates;
the second step, the preparation of canning slab, wherein, the used canning of canning slab includes the last titanium plate that both ends were bent and the lower titanium plate that both ends were bent (see fig. 2), and the side of canning is equipped with and is used for ventilative square hole, and commercial pure titanium is chooseed for use to upper and lower titanium plate, includes: firstly, alternately stacking Zr-Ta plates and Ti-Mo plates according to the sequence of Ti-Mo/Zr-Ta/Ti-Ta … … Ti-Mo/Zr-Ta/Ti-Mo (the stacking schematic diagram is shown in figure 1), stacking 21 layers, then coating glass lubricant on the surfaces of two Ti-Mo plates in contact with an upper titanium plate and a lower titanium plate of a sheath for lubrication, then placing the stacked Ti-Mo plates and Zr-Ta plates into the lower titanium plate, welding the upper titanium plate and the lower titanium plate in an argon arc welding mode, vacuumizing the sheath through a reserved square hole of the sheath (the vacuum degree is 0.1-1 Pa), and finally sealing the square hole by adopting high-temperature vacuum sealing mud to obtain a sheath plate blank;
thirdly, heating the sheathed plate blank to 600-700 ℃ by using a box type resistance furnace, and preserving heat for 20-30 min to finish preheating before extrusion; extruding and deforming the preheated sheathed plate blank on a 600-ton horizontal extruder at the speed of 15-25 mm/s; heating and insulating the sheathed plate blank by an electric induction heater arranged in an extrusion cylinder bushing in the extrusion process, wherein the extrusion temperature is controlled to be 400-500 ℃, and the extrusion ratio is 0.3-0.5;
fourthly, placing the extruded sheathed plate blank in a box type resistance furnace for heating, wherein the heating temperature is 500-600 ℃, and the temperature is kept for 10-30 min; after heating, putting the sheathed plate blank into a rolling mill for rolling for 3 passes, wherein the single-pass deformation is 60-70%, 55-65% and 45-55% in sequence, and the total rolling deformation is not lower than 90-95%; removing the sheath wrapped outside the stacked Ti-Mo plate and Zr-Ta plate after rolling, and carrying out acid washing and/or alcohol ultrasonic cleaning on the stacked Ti-Mo plate and Zr-Ta plate to obtain a Zr-Ta micron sheet reinforced Ti-Mo laminated composite plate, namely the Zr-Ta/Ti-Mo laminated composite plate with a submicron structure;
fifthly, cutting a raw material plate from the Zr-Ta/Ti-Mo laminated composite plate with the submicron structure obtained in the step by adopting a linear cutting and/or machining method, and obtaining the Zr-Ta/Ti-Mo laminated composite plate with the submicron structure and a fresh surface (without dirt or surface oxide skin) by mechanically polishing and ultrasonically cleaning the Zr-Ta/Ti-Mo laminated composite plate;
sixthly, the preparation second canning slab, wherein, the used second of second canning slab includes that both ends bend last iron plate and both ends bend lower iron plate (see fig. 2), and the side of second canning is equipped with and is used for ventilative square hole, and commercial pure iron is chooseed for use to upper and lower iron plate, includes: firstly, stacking 80-120 Zr-Ta/Ti-Mo laminated composite plates with submicron structures, then coating glass lubricant on the surfaces of two Zr-Ta/Ti-Mo laminated composite plates in contact with an upper iron plate and a lower iron plate of a second sheath for lubrication, putting the stacked Zr-Ta/Ti-Mo laminated composite plates into the lower iron plate, then welding the upper iron plate and the lower iron plate in an argon arc welding mode, vacuumizing the second sheath through a reserved square hole of the second sheath (the vacuum degree is 1-2 Pa), and finally sealing the square hole by adopting high-temperature vacuum sealing mud to obtain a second sheath plate blank;
seventhly, heating the second sheathing plate blank to 700-800 ℃ by using a box type resistance furnace, and preserving heat for 10-30 min to preheat before extrusion; extruding and deforming the preheated second sheath plate blank on a 600-ton horizontal extruder at the speed of 10-20 mm/s; heating and insulating the second sheathing board blank by an electric induction heater arranged in a bushing of an extrusion cylinder in the extrusion process, wherein the extrusion temperature is controlled to be 500-550 ℃, and the extrusion ratio is 0.3-0.5;
eighthly, placing the extruded second sheathing plate blank in a box-type resistance furnace for heating at the temperature of 550-650 ℃, and preserving heat for 10-30 min; after heating, putting the second sleeve plate blank into a rolling mill for rolling for 5 passes, wherein the single-pass deformation is 60-70%, 50-60%, 40-50% and 30-40% in sequence, and the total rolling deformation is not lower than 95-98%;
and ninthly, removing the sheath wrapped outside the composite board after rolling, carrying out acid cleaning and/or alcohol ultrasonic cleaning on the composite board, and then carrying out recrystallization annealing for 10-30 min at the temperature of 600-675 ℃, thereby obtaining the Zr-Ta nanosheet reinforced Ti-Mo (Zr-Ta/Ti-Mo) composite material.
The advantages of the invention include:
(1) the invention provides a Zr-Ta nanosheet reinforced Ti-Mo-based (abbreviated as Zr-Ta/Ti-Mo) composite material and a preparation method thereof, and the prepared Zr-Ta/Ti-Mo composite material realizes good matching of high strength (including high yield strength and high tensile strength) and large elongation rate on the premise of keeping a single BCC structure on the whole, and has important and wide application prospect in the high-technology fields of biomedicine, advanced industry and the like.
(2) The strength and the elongation of the composite material prepared by the invention can be designed and regulated based on the thickness ratio of the raw materials (namely Zr-Ta and Ti-Mo alloy) and the preparation process (such as slab manufacturing, hot extrusion, multi-pass rolling, heat treatment and other links), so that the composite material has good performance regulation and control characteristics. In addition, the Zr-Ta and Ti-Mo raw materials selected by the composite material prepared by the invention are both composed of non-cytotoxic elements, so that the composite material avoids potential cytotoxicity. In conclusion, the Zr-Ta/Ti-Mo composite material prepared by the invention not only can realize good matching of high strength and large elongation rate on the premise of keeping a single BCC structure, but also has excellent performance controllability and potential non-cytotoxicity characteristic.
In order to clearly understand the technical features, objects and advantages of the present invention, the following embodiments are provided to explain the technical solutions of the present invention in detail, but the scope of the present invention is not limited to the following embodiments.
Example 1:
the operation steps comprise:
(1) selecting raw materials, comprising:
reinforcing materials: selecting Zr70Ta30(wt.%) alloy;
base material: selecting Ti90Mo10(wt.%) alloy.
(2)Zr70Ta30Nanosheet reinforced Ti90Mo10Preparation of a base composite material comprising:
(ii) cutting and/or machining from Zr by wire70Ta30Alloy and Ti90Mo10Zr of 100mm by 50mm by 0.3mm in size was cut out of the alloy70Ta30And Ti of 100mm by 50mm by 1.7mm in size90Mo10Raw material plates, and Zr with fresh surface (without dirt or surface oxide skin) is obtained by mechanically grinding and ultrasonically cleaning the two raw material plates70Ta30And Ti90Mo10A plate material;
manufacturing the sheathed plate blank, wherein the sheath used for the sheathed plate blank comprises an upper titanium plate with two bent ends and a lower titanium plate with two bent ends (see figure 2), the side surface of the sheath is provided with a square hole for ventilation, and the upper titanium plate and the lower titanium plate adopt commercial pure titanium, which comprises the following steps: firstly, Ti90Mo10Plate and Zr70Ta30The plate is according to Ti90Mo10/Zr70Ta30/Ti90Mo10/Zr70Ta30……Ti90Mo10/Zr70Ta30/Ti90Mo10In a sequence of alternating stacks (schematic stacking as shown in FIG. 1), 21 layers are stacked, followed by two Ti plates in contact with the upper and lower titanium plates of the sheath90Mo10Coating glass lubricant on the surface of the plate for lubrication, and stacking the Ti90Mo10Plate and Zr70Ta30Placing the plate into a lower titanium plate, welding the upper titanium plate and the lower titanium plate together in an argon arc welding mode, vacuumizing the sheath through a square hole reserved in the sheath (the vacuum degree is 0.1Pa), and finally sealing the square hole by adopting high-temperature vacuum sealing mud to obtain a sheath plate blank;
thirdly, heating the sheathed plate blank to 600 ℃ by using a box type resistance furnace, and preserving heat for 20min to preheat before extrusion; extruding and deforming the preheated sheathed plate blank on a 600-ton horizontal extruder at the speed of 15 mm/s; heating and insulating the sheathed plate blank by an electric induction heater arranged in an extrusion cylinder bushing in the extrusion process, wherein the extrusion temperature is controlled at 400 ℃, and the extrusion ratio is 0.3;
fourthly, the extruded sheathed plate blank is placed in a box type resistance furnace to be heated at the temperature ofKeeping the temperature at 500 ℃ for 10 min; after heating, putting the sheathed plate blank into a rolling mill for rolling for 3 passes, wherein the single-pass deformation is 60 percent, 55 percent and 45 percent in sequence, and the total rolling deformation is not lower than 90 percent; removing Ti wrapped in the stack after rolling90Mo10Plate and Zr70Ta30Sheathing the outside of the plates and for stacked Ti90Mo10Plate and Zr70Ta30Pickling and/or alcohol ultrasonic cleaning the plate to obtain Zr70Ta30Micron sheet reinforced Ti90Mo10Layered composite plates, i.e. Zr with submicron structure70Ta30/Ti90Mo10A layered composite board;
adopting a linear cutting and/or machining method to obtain the Zr with the submicron structure70Ta30/Ti90Mo10Cutting a raw material plate on the laminated composite plate, and obtaining Zr with a fresh surface (without dirt or surface oxide skin) and a submicron structure by mechanically grinding and ultrasonically cleaning the raw material plate70Ta30/Ti90Mo10A layered composite board;
sixthly, make second wrap plate base, wherein, the used second wrap of second wrap plate base includes the last iron plate that both ends were bent and the lower iron plate that both ends were bent (see fig. 2), and the side of second wrap is equipped with and is used for ventilative square hole, and commercial pure iron is chooseed for use to upper and lower iron plate, includes: first 80 pieces of Zr with submicron structure70Ta30/Ti90Mo10The layered composite plates were stacked, followed by two pieces of Zr in contact with the upper and lower iron plates of the second clad70Ta30/Ti90Mo10Smearing glass lubricant on the surface of the layered composite board for lubrication, and stacking the Zr70Ta30/Ti90Mo10The layered composite plate is placed into the lower iron plate, then the upper iron plate and the lower iron plate are welded together in an argon arc welding mode, the second sheath is vacuumized through a reserved square hole of the second sheath (the vacuum degree is 1Pa), and finally the square hole is sealed by adopting high-temperature vacuum sealing mud to obtain a second sheath plate blank;
seventhly, heating the second wrapping plate blank to 700 ℃ by using a box type resistance furnace, preserving heat for 10min, and preheating before extrusion; extruding and deforming the preheated second sheath plate blank on a 600-ton horizontal extruder at the speed of 10 mm/s; heating and insulating the second sheathing board blank by an electric induction heater arranged in a bushing of an extrusion cylinder in the extrusion process, controlling the extrusion temperature at 500 ℃ and the extrusion ratio at 0.3;
eighthly, placing the extruded second clad plate blank in a box type resistance furnace to heat at 550 ℃ for 10 min; after heating, putting the second sleeve plate blank into a rolling mill for rolling for 5 passes, wherein the single-pass deformation is 60%, 50%, 50%, 40% and 30% in sequence, and the total rolling deformation is not lower than 95%;
ninthly, removing the sheath coated outside the composite board after rolling, carrying out acid cleaning and/or alcohol ultrasonic cleaning on the composite board, and then carrying out recrystallization annealing for 10min at 600 ℃ to obtain Zr70Ta30Nanosheet reinforced Ti90Mo10Radical (Zr)70Ta30/Ti90Mo10) A composite material.
(3) Alloy detection
Zr analysis by high-energy X-ray synchrotron radiation (HE-SXRD)70Ta30Nanosheet reinforced Ti90Mo10Radical (Zr)70Ta30/Ti90Mo10) Phase composition of composite Material synchrotron radiation testing Using 11-1D-C line station light Source from Argonne National Laboratory (Argonne National Laboratory), USA, with an experimental spot size of 0.6X 0.6mm2At a wavelength of
Figure BDA0003065361170000071
FIG. 3 shows Zr in this example70Ta30Nanosheet reinforced Ti90Mo10High energy X-ray diffraction patterns of the base composite. It can be seen that all diffraction peaks in the plot are from the BCC phase, indicating Zr70Ta30/Ti90Mo10The composite material exhibits a unitary BCC structure as a whole.
Scanning electronic display using FEI Nova Nano 450 field emissionMicro-mirror observes Zr70Ta30Nanosheet reinforced Ti90Mo10Radical (Zr)70Ta30/Ti90Mo10) The cross section appearance of the composite material is characterized in that the sample is sequentially subjected to inlaying, grinding and polishing treatment before the test. FIG. 4 shows Zr in this example70Ta30Nanosheet reinforced Ti90Mo10Scanning electron microscope photograph of the cross section of the base composite material. As can be seen, Zr70Ta30/Ti90Mo10The composite material consists of Zr70Ta30Nanosheets (bright bands in the figure) and Ti90Mo10The matrix (dark areas in the figure) constitutes, presenting a typical layered composite structure. Wherein, Zr70Ta30The average thickness of the nano-sheets is 100nm, Zr70Ta30Nanosheet in Zr70Ta30/Ti90Mo10The volume fraction of the composite material is 15%. In addition, it can be seen that Zr70Ta30Nanosheet and Ti90Mo10And adverse reactions such as eutectic crystal or precipitation do not exist at the interface of the matrix, and good metallurgical bonding is formed.
For Zr on an Instron-8801 type tensile tester70Ta30Nanosheet reinforced Ti90Mo10Radical (Zr)70Ta30/Ti90Mo10) The composite was subjected to a room temperature tensile test using tensile specimens along the Zr70Ta30/Ti90Mo10The standard dog-bone-shaped test sample cut from the original rolling direction of the composite material has a gauge length of 25mm, the surface and the section of the tensile test sample are required to be polished to remove oxide skin and cutting marks before the test, the strain value of the test sample in the tensile process is measured by an electronic extensometer in the test process, the strain rate is 1 multiplied by 10, and the strain rate is 1 multiplied by 10-3s-1. FIG. 5 shows Zr in this example70Ta30Nanosheet reinforced Ti90Mo10Stress-strain curves of the base composite during stretching. It can be seen that Zr70Ta30/Ti90Mo10The yield strength of the composite material is 721MPa, the tensile strength is 1308MPa, and the elongation is 38 percent, and the product of tensile strength and elongation reaches 49.7 GPa. This indicates Zr70Ta30/Ti90Mo10The composite material achieves good matching of high yield strength, high tensile strength and large elongation.
From the above tests and characterization, it can be found that Zr of the present example70Ta30Nanosheet reinforced Ti90Mo10The base composite material realizes good matching of high strength (including high yield strength and high tensile strength) and large elongation rate on the premise of keeping a single BCC structure, and is expected to be applied to the high-tech fields of biomedicine, advanced industry and the like. Zr of this example70Ta30Nanosheet reinforced Ti90Mo10The performance pair ratio of the matrix composite material to the existing beta titanium alloy is shown in table 1:
TABLE 1
Figure BDA0003065361170000081
As is clear from Table 1, Zr in the present example is compared with the conventional beta titanium alloy having a single BCC structure70Ta30Nanosheet reinforced Ti90Mo10The matrix composite not only has higher yield strength and tensile strength, but also has larger elongation and tensile strength-elongation product, and realizes good matching of high strength (including high yield strength and high tensile strength) and large elongation in the BCC structure.
Example 2:
the operation steps comprise:
(1) selecting raw materials, comprising:
reinforcing materials: selecting Zr60Ta40(wt.%) alloy;
base material: selecting Ti85Mo15(wt.%) alloy.
(2)Zr60Ta40Nanosheet reinforced Ti85Mo15Preparation of a base composite material comprising:
(ii) cutting and/or machining from Zr by wire60Ta40Alloy and Ti85Mo15Zr with the size of 120mm multiplied by 60mm multiplied by 0.4mm is respectively cut out of the alloy60Ta40And Ti of 120mm by 60mm by 1.6mm in size85Mo15Raw material plates, and Zr with fresh surface (without dirt or surface oxide skin) is obtained by mechanically grinding and ultrasonically cleaning the two raw material plates60Ta40And Ti85Mo15A plate material;
manufacturing the sheathed plate blank, wherein the sheath used for the sheathed plate blank comprises an upper titanium plate with two bent ends and a lower titanium plate with two bent ends (see figure 2), the side surface of the sheath is provided with a square hole for ventilation, and the upper titanium plate and the lower titanium plate adopt commercial pure titanium, which comprises the following steps: firstly, Ti85Mo15Plate and Zr60Ta40The plate is according to Ti85Mo15/Zr60Ta40/Ti85Mo15/Zr60Ta40……Ti85Mo15/Zr60Ta40/Ti85Mo15In a sequence of alternating stacks (schematic stacking as shown in FIG. 1), 21 layers are stacked, followed by two Ti plates in contact with the upper and lower titanium plates of the sheath85Mo15Coating glass lubricant on the surface of the plate for lubrication, and stacking the Ti85Mo15Plate and Zr60Ta40Placing the plate into a lower titanium plate, welding the upper titanium plate and the lower titanium plate together in an argon arc welding mode, vacuumizing the sheath through a square hole reserved in the sheath (the vacuum degree is 0.5Pa), and finally sealing the square hole by adopting high-temperature vacuum sealing mud to obtain a sheath plate blank;
thirdly, heating the sheathed plate blank to 650 ℃ by using a box type resistance furnace, and preserving heat for 25min to preheat before extrusion; extruding and deforming the preheated sheathed plate blank on a 600-ton horizontal extruder at the speed of 20 mm/s; heating and insulating the sheathed plate blank by an electric induction heater arranged in an extrusion cylinder bushing in the extrusion process, wherein the extrusion temperature is controlled at 450 ℃, and the extrusion ratio is 0.4;
fourthly, the extruded sheathed plate blank is placed in a box type resistance furnace to be heated, the heating temperature is 550 ℃, and the temperature is preserved for 20 min; after heating, putting the sheathed plate blank into a roller millRolling by the machine for 3 passes, wherein the single-pass deformation is 65%, 60% and 50% in sequence, and the total rolling deformation is not lower than 93%; removing Ti wrapped in the stack after rolling85Mo15Plate and Zr60Ta40Sheathing the outside of the plates and for stacked Ti85Mo15Plate and Zr60Ta40Pickling and/or alcohol ultrasonic cleaning the plate to obtain Zr60Ta40Micron sheet reinforced Ti85Mo15Layered composite plates, i.e. Zr with submicron structure60Ta40/Ti85Mo15A layered composite board;
adopting a linear cutting and/or machining method to obtain the Zr with the submicron structure60Ta40/Ti85Mo15Cutting a raw material plate on the laminated composite plate, and obtaining Zr with a fresh surface (without dirt or surface oxide skin) and a submicron structure by mechanically grinding and ultrasonically cleaning the raw material plate60Ta40/Ti85Mo15A layered composite board;
sixthly, make second wrap plate base, wherein, the used second wrap of second wrap plate base includes the last iron plate that both ends were bent and the lower iron plate that both ends were bent (see fig. 2), and the side of second wrap is equipped with and is used for ventilative square hole, and commercial pure iron is chooseed for use to upper and lower iron plate, includes: first 100 pieces of Zr with submicron structure60Ta40/Ti85Mo15The layered composite plates were stacked, followed by two pieces of Zr in contact with the upper and lower iron plates of the second clad60Ta40/Ti85Mo15Smearing glass lubricant on the surface of the layered composite board for lubrication, and stacking the Zr60Ta40/Ti85Mo15The layered composite plate is placed into the lower iron plate, then the upper iron plate and the lower iron plate are welded together in an argon arc welding mode, the second sheath is vacuumized through a reserved square hole of the second sheath (the vacuum degree is 1.5Pa), and finally the square hole is sealed by adopting high-temperature vacuum sealing mud to obtain a second sheath plate blank;
seventhly, heating the second sheathing plate blank to 750 ℃ by using a box type resistance furnace, preserving heat for 20min, and preheating before extrusion; extruding and deforming the preheated second sheath plate blank on a 600-ton horizontal extruder at the speed of 15 mm/s; heating and insulating the second sheathing board blank by an electric induction heater arranged in a bushing of the extrusion cylinder in the extrusion process, wherein the extrusion temperature is controlled at 525 ℃ and the extrusion ratio is 0.4;
placing the extruded second clad plate blank in a box type resistance furnace to heat at 600 ℃ for 20 min; after heating, putting the second sleeve plate blank into a rolling mill for rolling for 5 passes, wherein the single-pass deformation is 65%, 55%, 55%, 45% and 35% in sequence, and the total rolling deformation is not lower than 97%;
ninthly, removing the sheath coated outside the composite board after rolling, carrying out acid cleaning and/or alcohol ultrasonic cleaning on the composite board, and then carrying out recrystallization annealing for 20min at 640 ℃ to obtain Zr60Ta40Nanosheet reinforced Ti85Mo15Radical (Zr)60Ta40/Ti85Mo15) A composite material.
(3) Alloy detection
Zr analysis by high-energy X-ray synchrotron radiation (HE-SXRD)60Ta40Nanosheet reinforced Ti85Mo15Radical (Zr)60Ta40/Ti85Mo15) Phase composition of composite Material synchrotron radiation testing Using 11-1D-C line station light Source from Argonne National Laboratory (Argonne National Laboratory), USA, with an experimental spot size of 0.6X 0.6mm2At a wavelength of
Figure BDA0003065361170000101
FIG. 6 shows Zr in this example60Ta40Nanosheet reinforced Ti85Mo15High energy X-ray diffraction patterns of the base composite. It can be seen that all diffraction peaks in the plot are from the BCC phase, indicating Zr60Ta40/Ti85Mo15The composite material exhibits a unitary BCC structure as a whole.
Zr observation by FEI Nova Nano 450 field emission scanning electron microscope60Ta40Nano-sheetStrong Ti85Mo15Radical (Zr)60Ta40/Ti85Mo15) The cross section appearance of the composite material is characterized in that the sample is sequentially subjected to inlaying, grinding and polishing treatment before the test. FIG. 7 shows Zr in this example60Ta40Nanosheet reinforced Ti85Mo15Scanning electron microscope photograph of the cross section of the base composite material. As can be seen, Zr60Ta40/Ti85Mo15The composite material consists of Zr60Ta40Nanosheets (bright bands in the figure) and Ti85Mo15The matrix (dark areas in the figure) constitutes, presenting a typical layered composite structure. Wherein, Zr60Ta40The average thickness of the nano-sheet is 119nm, Zr60Ta40Nanosheet in Zr60Ta40/Ti85Mo15The volume fraction of the composite material is 19%. In addition, it can be seen that Zr60Ta40Nanosheet and Ti85Mo15And adverse reactions such as eutectic crystal or precipitation do not exist at the interface of the matrix, and good metallurgical bonding is formed.
For Zr on an Instron-8801 type tensile tester60Ta40Nanosheet reinforced Ti85Mo15Radical (Zr)60Ta40/Ti85Mo15) The composite was subjected to a room temperature tensile test using tensile specimens along the Zr60Ta40/Ti85Mo15The standard dog-bone-shaped test sample cut from the original rolling direction of the composite material has a gauge length of 25mm, the surface and the section of the tensile test sample are required to be polished to remove oxide skin and cutting marks before the test, the strain value of the test sample in the tensile process is measured by an electronic extensometer in the test process, the strain rate is 1 multiplied by 10, and the strain rate is 1 multiplied by 10-3s-1. FIG. 8 shows Zr in this example60Ta40Nanosheet reinforced Ti85Mo15Stress-strain curves of the base composite during stretching. It can be seen that Zr60Ta40/Ti85Mo15The yield strength of the composite material is 1020MPa, the tensile strength is 1452MPa, the elongation is 22 percent, and the product of the tensile strength and the elongation reaches 31.9 GPa. This is achieved byIndicates Zr60Ta40/Ti85Mo15The composite material achieves good matching of high yield strength, high tensile strength and large elongation.
From the above tests and characterization, it can be found that Zr of the present example60Ta40Nanosheet reinforced Ti85Mo15The base composite material realizes good matching of high strength (including high yield strength and high tensile strength) and large elongation rate on the premise of keeping a single BCC structure, and is expected to be applied to the high-tech fields of biomedicine, advanced industry and the like. Zr of this example60Ta40Nanosheet reinforced Ti85Mo15The property pair ratio of the base composite material and the existing beta-type titanium alloy is shown in table 2:
TABLE 2
Figure BDA0003065361170000111
As is clear from Table 2, Zr in the present example is compared with the conventional beta titanium alloy having a single BCC structure60Ta40Nanosheet reinforced Ti85Mo15The matrix composite not only has higher yield strength and tensile strength, but also has larger elongation and tensile strength-elongation product, and realizes good matching of high strength (including high yield strength and high tensile strength) and large elongation in the BCC structure.
Example 3:
the operation steps comprise:
(1) selecting raw materials, comprising:
reinforcing materials: selecting Zr50Ta50(wt.%) alloy;
base material: selecting Ti80Mo20(wt.%) alloy.
(2)Zr50Ta50Nanosheet reinforced Ti80Mo20Preparation of a base composite material comprising:
(ii) cutting and/or machining from Zr by wire50Ta50Alloy and Ti80Mo20The alloy was cut out of Zr having a size of 140mm X70 mm X0.5 mm50Ta50And Ti of 140mm by 70mm by 1.5mm in size80Mo20Raw material plates, and Zr with fresh surface (without dirt or surface oxide skin) is obtained by mechanically grinding and ultrasonically cleaning the two raw material plates50Ta50And Ti80Mo20A plate material;
manufacturing the sheathed plate blank, wherein the sheath used for the sheathed plate blank comprises an upper titanium plate with two bent ends and a lower titanium plate with two bent ends (see figure 2), the side surface of the sheath is provided with a square hole for ventilation, and the upper titanium plate and the lower titanium plate adopt commercial pure titanium, which comprises the following steps: firstly, Ti80Mo20Plate and Zr50Ta50The plate is according to Ti80Mo20/Zr50Ta50/Ti80Mo20/Zr50Ta50……Ti80Mo20/Zr50Ta50/Ti80Mo20In a sequence of alternating stacks (schematic stacking as shown in FIG. 1), 21 layers are stacked, followed by two Ti plates in contact with the upper and lower titanium plates of the sheath80Mo20Coating glass lubricant on the surface of the plate for lubrication, and stacking the Ti80Mo20Plate and Zr50Ta50Placing the plate into a lower titanium plate, welding the upper titanium plate and the lower titanium plate together in an argon arc welding mode, vacuumizing the sheath through a square hole reserved in the sheath (the vacuum degree is 1Pa), and finally sealing the square hole by adopting high-temperature vacuum sealing mud to obtain a sheath plate blank;
thirdly, heating the sheathed plate blank to 700 ℃ by using a box type resistance furnace, and preserving heat for 30min to preheat before extrusion; extruding and deforming the preheated sheathed plate blank on a 600-ton horizontal extruder at the speed of 25 mm/s; heating and insulating the sheathed plate blank by an electric induction heater arranged in an extrusion cylinder bushing in the extrusion process, wherein the extrusion temperature is controlled at 500 ℃, and the extrusion ratio is 0.5;
fourthly, the extruded sheathed plate blank is placed in a box type resistance furnace to be heated, the heating temperature is 600 ℃, and the temperature is kept for 30 min; after heating, putting the sheathed plate blank into a rolling mill for rolling for 3 passes, wherein the deformation of the single pass is orderly70 percent, 65 percent and 55 percent, and the rolling total deformation is not less than 95 percent; removing Ti wrapped in the stack after rolling80Mo20Plate and Zr50Ta50Sheathing the outside of the plates and for stacked Ti80Mo20Plate and Zr50Ta50Pickling and/or alcohol ultrasonic cleaning the plate to obtain Zr50Ta50Micron sheet reinforced Ti80Mo20Layered composite plates, i.e. Zr with submicron structure50Ta50/Ti80Mo20A layered composite board;
adopting a linear cutting and/or machining method to obtain the Zr with the submicron structure50Ta50/Ti80Mo20Cutting a raw material plate on the laminated composite plate, and obtaining Zr with a fresh surface (without dirt or surface oxide skin) and a submicron structure by mechanically grinding and ultrasonically cleaning the raw material plate50Ta50/Ti80Mo20A layered composite board;
sixthly, make second wrap plate base, wherein, the used second wrap of second wrap plate base includes the last iron plate that both ends were bent and the lower iron plate that both ends were bent (see fig. 2), and the side of second wrap is equipped with and is used for ventilative square hole, and commercial pure iron is chooseed for use to upper and lower iron plate, includes: first, 120 pieces of Zr with submicron structure50Ta50/Ti80Mo20The layered composite plates were stacked, followed by two pieces of Zr in contact with the upper and lower iron plates of the second clad50Ta50/Ti80Mo20Smearing glass lubricant on the surface of the layered composite board for lubrication, and stacking the Zr50Ta50/Ti80Mo20The layered composite plate is placed into the lower iron plate, then the upper iron plate and the lower iron plate are welded together in an argon arc welding mode, the second sheath is vacuumized through a reserved square hole of the second sheath (the vacuum degree is 2Pa), and finally the square hole is sealed by adopting high-temperature vacuum sealing mud to obtain a second sheath plate blank;
seventhly, heating the second wrapping plate blank to 800 ℃ by using a box type resistance furnace, preserving heat for 30min, and preheating before extrusion; extruding and deforming the preheated second sheath plate blank on a 600-ton horizontal extruder at the speed of 20 mm/s; heating and insulating the second sheathing board blank by an electric induction heater arranged in a bushing of the extrusion cylinder in the extrusion process, wherein the extrusion temperature is controlled at 550 ℃, and the extrusion ratio is 0.5;
placing the extruded second clad plate blank in a box type resistance furnace to heat at 650 ℃, and preserving heat for 30 min; after heating, putting the second sleeve plate blank into a rolling mill for rolling for 5 passes, wherein the single-pass deformation is 70%, 60%, 60%, 50% and 40% in sequence, and the total rolling deformation is not lower than 98%;
ninthly, removing the sheath coated outside the composite board after the rolling is finished, carrying out acid cleaning and/or alcohol ultrasonic cleaning on the composite board, and then carrying out recrystallization annealing for 30min at 675 ℃, thereby obtaining Zr50Ta50Nanosheet reinforced Ti80Mo20Radical (Zr)50Ta50/Ti80Mo20) A composite material.
(3) Alloy detection
Zr analysis by high-energy X-ray synchrotron radiation (HE-SXRD)50Ta50Nanosheet reinforced Ti80Mo20Radical (Zr)50Ta50/Ti80Mo20) Phase composition of composite Material synchrotron radiation testing Using 11-1D-C line station light Source from Argonne National Laboratory (Argonne National Laboratory), USA, with an experimental spot size of 0.4X 0.4mm2At a wavelength of
Figure BDA0003065361170000131
FIG. 9 shows Zr in this example50Ta50Nanosheet reinforced Ti80Mo20High energy X-ray diffraction patterns of the base composite. It can be seen that all diffraction peaks in the plot are from the BCC phase, indicating Zr50Ta50/Ti80Mo20The composite material exhibits a unitary BCC structure as a whole.
Zr observation by FEI Nova Nano 450 field emission scanning electron microscope50Ta50Nanosheet reinforced Ti80Mo20Radical (Zr)50Ta50/Ti80Mo20) The cross section appearance of the composite material is characterized in that the sample is sequentially subjected to inlaying, grinding and polishing treatment before the test. FIG. 10 shows Zr in this example50Ta50Nanosheet reinforced Ti80Mo20Scanning electron microscope photograph of the cross section of the base composite material. As can be seen, Zr50Ta50/Ti80Mo20The composite material consists of Zr50Ta50Nanosheets (bright bands in the figure) and Ti80Mo20The matrix (dark areas in the figure) constitutes, presenting a typical layered composite structure. Wherein, Zr50Ta50The average thickness of the nano-sheet is 93nm, Zr50Ta50Nanosheet in Zr50Ta50/Ti80Mo20The composite material accounts for 22% of the volume fraction. In addition, it can be seen that Zr50Ta50Nanosheet and Ti80Mo20And adverse reactions such as eutectic crystal or precipitation do not exist at the interface of the matrix, and good metallurgical bonding is formed.
For Zr on an Instron-8801 type tensile tester50Ta50Nanosheet reinforced Ti80Mo20Radical (Zr)50Ta50/Ti80Mo20) The composite was subjected to a room temperature tensile test using tensile specimens along the Zr50Ta50/Ti80Mo20The standard dog-bone-shaped test sample cut from the original rolling direction of the composite material has a gauge length of 25mm, the surface and the section of the tensile test sample are required to be polished to remove oxide skin and cutting marks before the test, the strain value of the test sample in the tensile process is measured by an electronic extensometer in the test process, the strain rate is 1 multiplied by 10, and the strain rate is 1 multiplied by 10-3s-1. FIG. 11 shows Zr in this example50Ta50Nanosheet reinforced Ti80Mo20Stress-strain curves of the base composite during stretching. It can be seen that Zr50Ta50/Ti80Mo20The yield strength of the composite material is 1023MPa, the tensile strength is 1428MPa, the elongation is 28 percent, and the product of the tensile strength and the elongation reaches 40.0 GPa. This indicates Zr50Ta50/Ti80Mo20The composite material achieves good matching of high yield strength, high tensile strength and large elongation.
From the above tests and characterization, it can be found that Zr of the present example50Ta50Nanosheet reinforced Ti80Mo20The base composite material realizes good matching of high strength (including high yield strength and high tensile strength) and large elongation rate on the premise of keeping a single BCC structure, and is expected to be applied to the high-tech fields of biomedicine, advanced industry and the like. Zr of this example50Ta50Nanosheet reinforced Ti80Mo20The property pair ratios of the base composite material and the existing beta titanium alloy are shown in table 3:
TABLE 3
Figure BDA0003065361170000141
As is clear from Table 3, Zr in the present example is compared with the conventional beta titanium alloy having a single BCC structure50Ta50Nanosheet reinforced Ti80Mo20The matrix composite not only has higher yield strength and tensile strength, but also has larger elongation and tensile strength-elongation product, and realizes good matching of high strength (including high yield strength and high tensile strength) and large elongation in the BCC structure.
Reference documents:
[1]W.J.Weng,A.Biesiekierski,J.X.Lin,S.Ozan,Y.C.Li,C.Wen,Development of beta-type Ti-Nb-Zr-Mo alloys for orthopedic applications,Applied Materials Today 22(2021)100968.
[2]A.Ramarolahy,P.Castany,T.Gloriant,F.Prima,P.Laheurte,A.Eberhardt,E.Patoor,Synthesis and characterisation of new superelastic and low elastic modulus Ti-Nb-X alloys for biomedical application,Advanced Materials Research 409(2012)170-174.
[3]J.I.Qazi,B.Marquardt,H.J.Rack,High-strength metastable beta-titanium alloys for biomedical applications,JOM 56(2004)49-51.
[4]M.Geetha,A.K.Singh,R.Asokamani,A.K.Gogia,Ti based biomaterials,the ultimate choice for orthopaedic implants-A review,Progress in Materials Science 54(2009)397-425.
[5]C.J.Cowen,C.J.Boehlert,The microstructure,creep,and tensile behavior for Ti-5Al-45Nb(atomic percent)fully-βalloy,Metallurgical and Materials Transactions A 38(2007)2747-2753.
[6]V.D.Cojocaru,A.Nocivin,C.Trisca-Rusu,A.Dan,R.Irimescu,D.Raducanu,B.M.Galbinasu,Improving the mechanical properties of aβ-type Ti-Nb-Zr-Fe-O alloy,Metals 10(2020)1491.

Claims (6)

  1. the preparation method of the Zr-Ta nanosheet reinforced Ti-Mo-based composite material is characterized by comprising the following steps of:
    A) alternately stacking Zr-Ta plates and Ti-Mo plates in the order of Ti-Mo/Zr-Ta/Ta … … Ti-Mo/Zr-Ta/Ti-Mo for 21 layers, wherein the Zr-Ta plates are Zr-Ta plates with Ta content of 30-50 wt% and sizes of (100 + 140mm) × (50-70mm) × (0.3-0.5mm), the Ti-Mo plates are Ti-Mo plates with Mo content of 10-20 wt% and sizes of (100 + 140mm) × (50-70mm) × (1.7-1.5mm),
    placing the stacked Ti-Mo plates and Zr-Ta plates into a sheath, welding an upper titanium plate and a lower titanium plate in an argon arc welding mode, vacuumizing the sheath to a vacuum degree range of 0.1-1 Pa through a square hole reserved in the sheath, and finally sealing the square hole by adopting high-temperature vacuum sealing mud to obtain a sheath plate blank, wherein the sheath comprises the upper titanium plate with two bent ends and the lower titanium plate with two bent ends, the side surface of the sheath is provided with the square hole, and the upper titanium plate and the lower titanium plate both adopt commercial pure titanium;
    B) heating the sheathed plate blank to 600-700 ℃, preserving heat for 20-30 min, and preheating before extrusion; extruding and deforming the preheated sheathed plate blank on a 600-ton horizontal extruder at the speed of 15-25 mm/s; heating and insulating the sheathed plate blank by an electric induction heater arranged in an extrusion cylinder bushing in the extrusion process, wherein the extrusion temperature is controlled to be 400-500 ℃, and the extrusion ratio is 0.3-0.5;
    C) heating the extruded sheathed plate blank in a box type resistance furnace at 500-600 ℃ for 10-30 min; after heating, putting the sheathed plate blank into a rolling mill for rolling for 3 passes, wherein the single-pass deformation is 60-70%, 55-65% and 45-55% in sequence, and the total rolling deformation is not lower than 90-95%; after rolling is finished, removing the sheath wrapped outside the stacked Ti-Mo plate and Zr-Ta plate to obtain a Zr-Ta micron sheet reinforced Ti-Mo laminated composite plate, namely a Zr-Ta/Ti-Mo laminated composite plate with a submicron structure;
    D) cutting a raw material plate from the Zr-Ta/Ti-Mo laminated composite plate with the submicron structure obtained by the steps by adopting a linear cutting and/or machining method, and obtaining the Zr-Ta/Ti-Mo laminated composite plate with a fresh surface and the submicron structure by carrying out mechanical polishing and ultrasonic cleaning on the raw material plate;
    E) the preparation second canning slab, wherein, the used second canning of second canning slab includes the last iron plate that both ends were bent and the lower iron plate that both ends were bent, and the side of second canning is equipped with and is used for ventilative square hole, and commercial pure iron is chooseed for use to iron plate from top to bottom, includes: firstly, stacking 80-120 Zr-Ta/Ti-Mo laminated composite plates with submicron structures, putting the stacked Zr-Ta/Ti-Mo laminated composite plates into a lower iron plate, welding an upper iron plate and the lower iron plate in an argon arc welding mode, vacuumizing a sheath to a vacuum degree range of 1-2 Pa through a reserved square hole of the sheath, and finally sealing the square hole by adopting high-temperature vacuum sealing mud to obtain a second sheath plate blank;
    F) heating the second sheathing plate blank to 700-800 ℃ by using a box type resistance furnace, preserving heat for 10-30 min, and preheating before extrusion; extruding and deforming the preheated second sheath plate blank on a 600-ton horizontal extruder at the speed of 10-20 mm/s; heating and insulating the second sheathing board blank by an electric induction heater arranged in a bushing of an extrusion cylinder in the extrusion process, wherein the extrusion temperature is controlled to be 500-550 ℃, and the extrusion ratio is 0.3-0.5;
    G) heating the extruded second sheathing plate blank in a box-type resistance furnace at 550-650 ℃, and preserving heat for 10-30 min; after heating, putting the second sleeve plate blank into a rolling mill for rolling for 5 passes, wherein the single-pass deformation is 60-70%, 50-60%, 40-50% and 30-40% in sequence, and the total rolling deformation is not lower than 95-98%;
    H) after rolling, removing the sheath wrapped outside the composite board, carrying out acid cleaning and/or alcohol ultrasonic cleaning on the composite board, and then carrying out recrystallization annealing on the composite board for 10-30 min at the temperature of 600-675 ℃, thereby obtaining the Zr-Ta nanosheet reinforced Ti-Mo based composite material.
  2. 2. The method for preparing a Zr-Ta nanosheet-reinforced Ti-Mo-based composite material according to claim 1, wherein:
    the Zr-Ta plate and the Ti-Mo plate are Zr-Ta and Ti-Mo plates respectively obtained by cutting from Zr-Ta alloy and Ti-Mo alloy by adopting a linear cutting and/or machining method,
    and the Zr-Ta and Ti-Mo plates are subjected to mechanical polishing and ultrasonic cleaning, so that the Zr-Ta and Ti-Mo plates with fresh surfaces are obtained.
  3. 3. The method for preparing a Zr-Ta nanosheet-reinforced Ti-Mo-based composite material according to claim 1, wherein:
    before the stacked Ti-Mo plates and Zr-Ta plates are put into the sheath, the surfaces of the two Ti-Mo plates which are in contact with the upper titanium plate and the lower titanium plate of the sheath of the stacked Ti-Mo plates and Zr-Ta plates are coated with glass lubricant for lubrication, and
    before the stacked Zr-Ta/Ti-Mo laminated composite board is placed in the lower iron plate, glass lubricant is coated on the surfaces of the two Zr-Ta/Ti-Mo plates, which are in contact with the upper iron plate and the lower iron plate of the second cladding sleeve, of the stacked Zr-Ta/Ti-Mo laminated composite board for lubrication.
  4. 4. The method for preparing a Zr-Ta nanosheet-reinforced Ti-Mo-based composite material according to claim 1, wherein:
    and in the step B), the sheathed plate blank is heated to 600-700 ℃ and is kept warm for 20-30 min by using a box type resistance furnace.
  5. 5. The method for preparing a Zr-Ta nanosheet-reinforced Ti-Mo-based composite material according to claim 1, wherein:
    and after removing the sheath wrapped outside the stacked Ti-Mo plate and the stacked Zr-Ta plate, carrying out acid washing and/or alcohol ultrasonic cleaning on the stacked Ti-Mo plate and the stacked Zr-Ta plate.
  6. 6. The Zr-Ta nanosheet-reinforced Ti-Mo-based composite material prepared by the preparation method according to any one of claims 1 to 5.
CN202110533591.9A 2021-05-13 2021-05-13 Zr-Ta nanosheet reinforced Ti-Mo-based composite material and preparation method thereof Active CN113634989B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110533591.9A CN113634989B (en) 2021-05-13 2021-05-13 Zr-Ta nanosheet reinforced Ti-Mo-based composite material and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110533591.9A CN113634989B (en) 2021-05-13 2021-05-13 Zr-Ta nanosheet reinforced Ti-Mo-based composite material and preparation method thereof

Publications (2)

Publication Number Publication Date
CN113634989A true CN113634989A (en) 2021-11-12
CN113634989B CN113634989B (en) 2022-11-04

Family

ID=78415866

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110533591.9A Active CN113634989B (en) 2021-05-13 2021-05-13 Zr-Ta nanosheet reinforced Ti-Mo-based composite material and preparation method thereof

Country Status (1)

Country Link
CN (1) CN113634989B (en)

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101144159A (en) * 2007-10-31 2008-03-19 上海工程技术大学 Method for preparing nano/submicron TiB-TiC enhanced titanium-base composite material (TiB+TiC)/Ti
US20100303722A1 (en) * 2006-06-23 2010-12-02 Sungho Jin Articles comprising large-surface-area bio-compatible materials and methods for making and using them
CN102899528A (en) * 2012-10-24 2013-01-30 中南大学 Biomedical beta-titanium alloy material and preparation method
CN105013821A (en) * 2015-07-02 2015-11-04 哈尔滨工程大学 Accumulative roll-bonding preparation method of nanometer lamellar phase enhanced TiNi alloy composite plate
CN105080999A (en) * 2015-09-16 2015-11-25 哈尔滨工业大学 Method for manufacturing TiAl/Ti alloy laminated composite plates in preheating pressing compositing and wrapping hot rolling manner
FR3047489A1 (en) * 2016-02-08 2017-08-11 Abdelmadjid Djemai PROCESS FOR MANUFACTURING A TITANIUM NIKIUM ZIRCONIUM (TNZ) BETA-ALLOY WITH A VERY LOW ELASTICITY MODULE FOR BIOMEDICAL APPLICATIONS AND ITS ADDITIVE FABRICATION EMBODIMENT
CN109706415A (en) * 2019-01-25 2019-05-03 北京工业大学 A kind of memory alloy-based nano lamellar composite material and preparation method
CN110284089A (en) * 2019-07-31 2019-09-27 上海交通大学 It is a kind of it is micro-/receive the isothermal superplastic deformation method of granule intensified titanium-base compound material

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100303722A1 (en) * 2006-06-23 2010-12-02 Sungho Jin Articles comprising large-surface-area bio-compatible materials and methods for making and using them
CN101144159A (en) * 2007-10-31 2008-03-19 上海工程技术大学 Method for preparing nano/submicron TiB-TiC enhanced titanium-base composite material (TiB+TiC)/Ti
CN102899528A (en) * 2012-10-24 2013-01-30 中南大学 Biomedical beta-titanium alloy material and preparation method
CN105013821A (en) * 2015-07-02 2015-11-04 哈尔滨工程大学 Accumulative roll-bonding preparation method of nanometer lamellar phase enhanced TiNi alloy composite plate
CN105080999A (en) * 2015-09-16 2015-11-25 哈尔滨工业大学 Method for manufacturing TiAl/Ti alloy laminated composite plates in preheating pressing compositing and wrapping hot rolling manner
FR3047489A1 (en) * 2016-02-08 2017-08-11 Abdelmadjid Djemai PROCESS FOR MANUFACTURING A TITANIUM NIKIUM ZIRCONIUM (TNZ) BETA-ALLOY WITH A VERY LOW ELASTICITY MODULE FOR BIOMEDICAL APPLICATIONS AND ITS ADDITIVE FABRICATION EMBODIMENT
CN109706415A (en) * 2019-01-25 2019-05-03 北京工业大学 A kind of memory alloy-based nano lamellar composite material and preparation method
CN110284089A (en) * 2019-07-31 2019-09-27 上海交通大学 It is a kind of it is micro-/receive the isothermal superplastic deformation method of granule intensified titanium-base compound material

Also Published As

Publication number Publication date
CN113634989B (en) 2022-11-04

Similar Documents

Publication Publication Date Title
TWI589704B (en) Thermo-mechanical processing of nickel-titanium alloys
CN105013821B (en) Nanoscale twins mutually strengthen the accumulation ply rolling preparation method of TiNi based alloy composite boards
Hausöl et al. Tailoring materials properties by accumulative roll bonding
CN100496817C (en) Method for preparing TiAl alloy clad plate by pre-alloying powder
EP1144704A1 (en) Damage tolerant aluminium alloy product and method of its manufacture
JPS5938295B2 (en) Superplastic aluminum alloy material and its manufacturing method
Zhang et al. Effects of annealing time on the microstructures and tensile properties of formed laminated composites in Ti-Ni system
CN110576072B (en) Preparation method of multilayer pure copper-brass composite board
CN105525236B (en) A kind of deformation heat treatment method of refining aluminum alloy crystal grain
Shuai et al. Effect of annealing temperature on microstructure and mechanical properties of cold-rolled commercially pure titanium sheets
DEHGHAN et al. Effect of inter-cycle heat treatment in accumulative roll-bonding (ARB) process on planar isotropy of mechanical properties of AA1050 sheets
CN105603258A (en) High-strength zirconium alloy and preparation method
CN110306137A (en) A kind of preparation method of stratiform copper chromium zirconium-fine copper composite board
Huang et al. Formability improvement of hot-pressed Ti/Al laminated sheet by TiAl3 layer growth and crack healing during deformation
CN113634989B (en) Zr-Ta nanosheet reinforced Ti-Mo-based composite material and preparation method thereof
NO333617B1 (en) Two-phase titanium aluminide alloy
CN117737548A (en) High-ductility cobalt-chromium-based alloy for biomedical capillary and preparation method thereof
CN116791014A (en) Biocompatible TiZrNbAl refractory high-entropy alloy with improved corrosion resistance in simulated body fluid by nanosecond laser shock peening
CN112853230B (en) Low-layer-dislocation-energy face-centered cubic structure high-entropy shape memory alloy and preparation method thereof
CN113715429B (en) Biomedical NiTiFe-Ta composite board and preparation method thereof
EP3878997A1 (en) Method of forming precursor into a ti alloy article
CN113564421A (en) High-strength corrosion-resistant zirconium alloy and preparation method and application thereof
Tsuji Accumulative roll-bonding
CN113352707A (en) TiMo-NiTi large-class linear elastic composite board and preparation method thereof
CN112063892A (en) High-thermal-stability equiaxial nanocrystalline Ti-Zr-Mn alloy and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant