CN113634989B - 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

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CN113634989B
CN113634989B CN202110533591.9A CN202110533591A CN113634989B CN 113634989 B CN113634989 B CN 113634989B CN 202110533591 A CN202110533591 A CN 202110533591A CN 113634989 B CN113634989 B CN 113634989B
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CN113634989A (en
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郭顺
黄豪
张慧慧
丁旺
沈宝国
刘海霞
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Jiangsu University
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    • 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

Abstract

The Zr-Ta nanosheet reinforced Ti-Mo-based (abbreviated as Zr-Ta/Ti-Mo) composite material and the preparation method thereof are provided, 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 in the single BCC structure, and can be expected to be applied to the high-tech 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, and are known as "triphibian metals in sea, land and air", due to their excellent comprehensive mechanical properties (high specific strength), good functional characteristics (shape memory and superelasticity), and excellent biocompatibility and corrosion resistance. 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 volume content of the omega phase in the titanium alloy exceeds 30%, the titanium alloy no longer has the characteristic of low elastic modulus, and the tensile elongation of the titanium alloy is reduced to 3%, which is about 1/7 of that of the 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 invention 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 High energy X-ray diffraction patterns of the base composite.
FIG. 4 shows Zr prepared according to example 1 of the present invention 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 Scanning electron microscope photograph of the cross section of the base composite material.
FIG. 5 shows Zr prepared according to example 1 of the present invention 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 Stress-strain curves of the base composite during stretching.
FIG. 6 shows Zr prepared according to example 2 of the present invention 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 High energy X-ray diffraction patterns of the base composite.
FIG. 7 shows a hair dryer according to the inventionZr prepared in Bright example 2 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 Scanning electron microscope photograph of the cross section of the base composite material.
FIG. 8 shows Zr prepared according to example 2 of the present invention 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 Stress-strain curves of the base composite during stretching.
FIG. 9 shows Zr prepared according to example 3 of the present invention 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 High energy X-ray diffraction patterns of the base composite.
FIG. 10 shows Zr prepared according to example 3 of the present invention 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 Scanning electron microscope photograph of the cross section of the base composite material.
FIG. 11 shows Zr prepared according to example 3 of the present invention 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 Stress-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: ti-Mo alloy (wherein the mass percent 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 plate blank, wherein, the used canning of canning plate blank 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-Mo/Zr-Ta … … Ti-Mo/Zr-Ta/Ti-Mo (a stacking schematic diagram is shown in figure 1), stacking 21 layers in total, 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 with reserved square holes of the sheath (the vacuum degree range is 0.1-1 Pa), and finally sealing the square holes by adopting high-temperature vacuum sealing mud to obtain a plate sheath;
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, the extruded sheathed plate blank is placed in a box-type resistance furnace to be heated, 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 previous 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 grinding and ultrasonically cleaning the raw material 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 clad 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 at 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 (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 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 proportion 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 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.
The technical features, objects and advantages of the present invention will be more clearly understood through the following examples, but the scope of the present invention is not limited to the following examples.
Example 1:
the operation steps comprise:
(1) Selecting raw materials, comprising:
reinforcing materials: selecting Zr 70 Ta 30 (wt.%) alloy;
base material: selecting Ti 90 Mo 10 (wt.%) alloy.
(2)Zr 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 Preparation of a base composite material comprising:
(1) from Zr by wire-cutting and/or machining 70 Ta 30 Alloy and Ti 90 Mo 10 Zr of 100mm by 50mm by 0.3mm in size was cut out of the alloy 70 Ta 30 And Ti of 100mm X50 mm X1.7 mm in size 90 Mo 10 Raw 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 plates 70 Ta 30 And Ti 90 Mo 10 A plate material;
(2) 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: first, ti 90 Mo 10 Plate and Zr 70 Ta 30 The plate is according to Ti 90 Mo 10 /Zr 70 Ta 30 /Ti 90 Mo 10 /Zr 70 Ta 30 ……Ti 90 Mo 10 /Zr 70 Ta 30 /Ti 90 Mo 10 In 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 sheath 90 Mo 10 Coating glass lubricant on the surface of the plate for lubrication, and stacking the Ti 90 Mo 10 Plate and Zr 70 Ta 30 Placing 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 0.1 Pa), and finally sealing the square hole by adopting high-temperature vacuum sealing mud to obtain a sheath plate blank;
(3) 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; in the extrusion process, the sheathed slab is heated and insulated by an electric induction heater arranged in an extrusion cylinder bushing, the extrusion temperature is controlled at 400 ℃, and the extrusion ratio is 0.3;
(4) heating the extruded sheathed plate blank in a box-type resistance furnace at 500 deg.C for 10min; 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 rolling 90 Mo 10 Plate and Zr 70 Ta 30 Sheathing of the outside of the plates, and of stacked Ti 90 Mo 10 Plate and Zr 70 Ta 30 Pickling and/or alcohol ultrasonic cleaning the plate to obtain Zr 70 Ta 30 Micron sheet reinforced Ti 90 Mo 10 Layered composite plates, i.e. Zr with submicron structure 70 Ta 30 /Ti 90 Mo 10 A layered composite board;
(5) from Zr having submicron structure obtained by the above steps by wire cutting and/or machining 70 Ta 30 /Ti 90 Mo 10 Cutting raw material plate on the laminated composite board and feeding the raw material plateMechanical grinding and ultrasonic cleaning to obtain Zr with submicron structure and fresh surface (without dirt or surface scale) 70 Ta 30 /Ti 90 Mo 10 A layered composite board;
(6) make second canning slab, wherein, the used second of second canning slab overlaps including 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 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: first 80 pieces of Zr with submicron structure 70 Ta 30 /Ti 90 Mo 10 The layered composite plates were stacked, followed by two pieces of Zr in contact with the upper and lower iron plates of the second clad 70 Ta 30 /Ti 90 Mo 10 Smearing glass lubricant on the surface of the layered composite board for lubrication, and stacking the Zr 70 Ta 30 /Ti 90 Mo 10 The 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 Pa), and finally the square hole is sealed by adopting high-temperature vacuum sealing mud to obtain a second sheath plate blank;
(7) heating the second sheathing 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;
(8) heating the extruded second sheathing plate blank in a box-type resistance furnace at 550 ℃ for 10min; 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%;
(9) removing the sheath coated outside the composite board after rolling, performing acid cleaning and/or alcohol ultrasonic cleaning on the composite board, and performing recrystallization annealing at 600 deg.C for 10min to obtain the final productObtaining Zr 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 Radical (Zr) 70 Ta 30 /Ti 90 Mo 10 ) A composite material.
(3) Alloy detection
Zr analysis by high-energy X-ray synchrotron radiation (HE-SXRD) 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 Radical (Zr) 70 Ta 30 /Ti 90 Mo 10 ) 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 0.6mm 2 At a wavelength of
Figure BDA0003065361170000071
FIG. 3 shows Zr in this example 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 High 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 Zr 70 Ta 30 /Ti 90 Mo 10 The composite material exhibits a unitary BCC structure as a whole.
Zr is observed by using a FEI Nova Nano 450 field emission scanning electron microscope 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 Radical (Zr) 70 Ta 30 /Ti 90 Mo 10 ) 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 example 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 Scanning electron microscope photograph of the cross section of the base composite material. As can be seen, zr 70 Ta 30 /Ti 90 Mo 10 The composite material consists of Zr 70 Ta 30 Nanosheets (bright bands in the figure) and Ti 90 Mo 10 The matrix (dark areas in the figure) constitutes, presenting a typical layered composite structure. Wherein, zr 70 Ta 30 The average thickness of the nanosheets is 100nm 70 Ta 30 Nanosheet in Zr 70 Ta 30 /Ti 90 Mo 10 The volume fraction of the composite material is 15%. In addition, in the case of the present invention,it can also be seen that Zr 70 Ta 30 Nanosheet and Ti 90 Mo 10 And 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 tester 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 Radical (Zr) 70 Ta 30 /Ti 90 Mo 10 ) The composite was subjected to a room temperature tensile test using tensile specimens along the Zr 70 Ta 30 /Ti 90 Mo 10 The gauge length of a standard dog-bone-shaped sample cut from the original rolling direction of the composite material is 25mm, the surface and the cross section of a tensile sample are required to be polished to remove oxide skin and cutting marks before a test, the strain value of the 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 -3 s -1 . FIG. 5 shows Zr in this example 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 Stress-strain curves of the base composite during stretching. It can be seen that Zr 70 Ta 30 /Ti 90 Mo 10 The yield strength of the composite material is 721MPa, the tensile strength is 1308MPa, the elongation is 38 percent, and the product of the tensile strength and the elongation reaches 49.7 GPa. This indicates Zr 70 Ta 30 /Ti 90 Mo 10 The 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 example 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 The 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 example 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 The 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 structure 70 Ta 30 Nanosheet reinforced Ti 90 Mo 10 The 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, including:
reinforcing materials: selecting Zr 60 Ta 40 (wt.%) alloy;
base material: selecting Ti 85 Mo 15 (wt.%) alloy.
(2)Zr 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 Preparation of a base composite material comprising:
(1) from Zr by wire-cutting and/or machining 60 Ta 40 Alloy and Ti 85 Mo 15 Zr with the size of 120mm multiplied by 60mm multiplied by 0.4mm is respectively cut out of the alloy 60 Ta 40 And Ti of 120mm by 60mm by 1.6mm in size 85 Mo 15 Raw 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 plates 60 Ta 40 And Ti 85 Mo 15 A plate material;
(2) 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, ti 85 Mo 15 Plate and Zr 60 Ta 40 The plate is according to Ti 85 Mo 15 /Zr 60 Ta 40 /Ti 85 Mo 15 /Zr 60 Ta 40 ……Ti 85 Mo 15 /Zr 60 Ta 40 /Ti 85 Mo 15 In 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 sheath 85 Mo 15 Coating glass lubricant on the surface of the plate for lubrication, and stacking the Ti 85 Mo 15 Plate and Zr 60 Ta 40 Placing 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 0.5 Pa), and finally sealing the square hole by adopting high-temperature vacuum sealing mud to obtain a sheath plate blank;
(3) 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 jacketed plate blank on a 600-ton horizontal extruder at the speed of 20 mm/s; in the extrusion process, the sheathed slab is heated and insulated by an electric induction heater arranged in an extrusion cylinder bush, the extrusion temperature is controlled at 450 ℃, and the extrusion ratio is 0.4;
(4) heating the extruded sheathed plate blank in a box-type resistance furnace at 550 ℃ for 20min; after heating, putting the sheathed plate blank into a rolling mill for rolling for 3 passes, wherein the single-pass deformation is 65 percent, 60 percent and 50 percent in sequence, and the total rolling deformation is not lower than 93 percent; removing Ti wrapped in the stack after rolling 85 Mo 15 Plate and Zr 60 Ta 40 Sheathing the outside of the plates and for stacked Ti 85 Mo 15 Plate and Zr 60 Ta 40 Pickling and/or ultrasonically cleaning the board with alcohol to obtain Zr 60 Ta 40 Micron sheet reinforced Ti 85 Mo 15 Layered composite plates, i.e. Zr with submicron structure 60 Ta 40 /Ti 85 Mo 15 A layered composite board;
(5) from Zr having submicron structure obtained by the above steps by wire cutting and/or machining 60 Ta 40 /Ti 85 Mo 15 Cutting raw material plates on the laminated composite plate, and obtaining the laminated composite plate with a fresh surface by mechanically polishing and ultrasonically cleaning the laminated composite plateSurface (no fouling or surface scale) Zr with submicron structure 60 Ta 40 /Ti 85 Mo 15 A layered composite board;
(6) make second canning slab, wherein, the used second of second canning slab overlaps including 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 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: first 100 pieces of Zr with submicron structure 60 Ta 40 /Ti 85 Mo 15 The layered composite plates were stacked, followed by two pieces of Zr in contact with the upper and lower iron plates of the second clad 60 Ta 40 /Ti 85 Mo 15 Smearing glass lubricant on the surface of the layered composite board for lubrication, and stacking the Zr 60 Ta 40 /Ti 85 Mo 15 The 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 1.5 Pa), and finally the square hole is sealed by adopting high-temperature vacuum sealing mud to obtain a second sheath plate blank;
(7) 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;
(8) heating the extruded second sheathing board blank in a box-type resistance furnace at 600 ℃ for 20min; 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%;
(9) 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 at 640 ℃ for 20min to obtain Zr 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 Radical (Zr) 60 Ta 40 /Ti 85 Mo 15 ) A composite material.
(3) Alloy detection
Zr analysis by high-energy X-ray synchrotron radiation (HE-SXRD) 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 Radical (Zr) 60 Ta 40 /Ti 85 Mo 15 ) 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 0.6mm 2 At a wavelength of
Figure BDA0003065361170000101
FIG. 6 shows Zr in this example 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 High 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 Zr 60 Ta 40 /Ti 85 Mo 15 The composite material exhibits a unitary BCC structure as a whole.
Zr observation by FEI Nova Nano 450 field emission scanning electron microscope 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 Radical (Zr) 60 Ta 40 /Ti 85 Mo 15 ) 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 example 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 Scanning electron microscope photograph of the cross section of the base composite material. As can be seen, zr 60 Ta 40 /Ti 85 Mo 15 The composite material consists of Zr 60 Ta 40 Nanosheets (bright bands in the figure) and Ti 85 Mo 15 The matrix (dark areas in the figure) constitutes, presenting a typical layered composite structure. Wherein, zr 60 Ta 40 The average thickness of the nanosheets is 119nm 60 Ta 40 Nanosheet in Zr 60 Ta 40 /Ti 85 Mo 15 The volume fraction of the composite material is 19 percent. In addition, it can be seen that Zr 60 Ta 40 Nano meterSheet and Ti 85 Mo 15 And 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 tester 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 Radical (Zr) 60 Ta 40 /Ti 85 Mo 15 ) The composite was subjected to a room temperature tensile test using tensile specimens along the Zr 60 Ta 40 /Ti 85 Mo 15 The 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 -3 s -1 . FIG. 8 shows Zr in this example 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 Stress-strain curves of the base composite during stretching. It can be seen that Zr 60 Ta 40 /Ti 85 Mo 15 The 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 indicates Zr 60 Ta 40 /Ti 85 Mo 15 The 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 example 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 The 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 example 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 The performance ratio of the matrix composite material to the existing beta 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 structure 60 Ta 40 Nanosheet reinforced Ti 85 Mo 15 The 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, including:
reinforcing materials: selecting Zr 50 Ta 50 (wt.%) alloy;
base material: selecting Ti 80 Mo 20 (wt.%) alloy.
(2)Zr 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 Preparation of a base composite material comprising:
(1) from Zr by wire-cutting and/or machining 50 Ta 50 Alloy and Ti 80 Mo 20 The alloy was cut out of Zr having a size of 140mm X70 mm X0.5 mm 50 Ta 50 And Ti of 140mm by 70mm by 1.5mm in size 80 Mo 20 Raw 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 plates 50 Ta 50 And Ti 80 Mo 20 A plate material;
(2) 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: first, ti 80 Mo 20 Plate and Zr 50 Ta 50 The plate is according to Ti 80 Mo 20 /Zr 50 Ta 50 /Ti 80 Mo 20 /Zr 50 Ta 50 ……Ti 80 Mo 20 /Zr 50 Ta 50 /Ti 80 Mo 20 In 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 sheath 80 Mo 20 The surface of the plate is coated with glass lubricant for lubrication, and then the stacked Ti is treated 80 Mo 20 Plate and Zr 50 Ta 50 Placing 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 the reserved square holes of the sheath (the vacuum degree is 1 Pa), and finally sealing the square holes by adopting high-temperature vacuum sealing mud to obtain a sheath plate blank;
(3) heating the sheathed plate blank to 700 ℃ by using a box type resistance furnace, preserving heat for 30min, and preheating 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;
(4) heating the extruded sheathed plate blank in a box-type resistance furnace at 600 deg.C for 30min; after heating, putting the sheathed plate blank into a rolling mill for rolling for 3 passes, wherein the single-pass deformation is 70 percent, 65 percent and 55 percent in sequence, and the total rolling deformation is not lower than 95 percent; removing Ti wrapped in the stack after rolling 80 Mo 20 Plate and Zr 50 Ta 50 Sheathing the outside of the plates and for stacked Ti 80 Mo 20 Plate and Zr 50 Ta 50 Pickling and/or alcohol ultrasonic cleaning the plate to obtain Zr 50 Ta 50 Micron sheet reinforced Ti 80 Mo 20 Layered composite plates, i.e. Zr with submicron structure 50 Ta 50 /Ti 80 Mo 20 A layered composite board;
(5) from Zr having submicron structure obtained by the above steps by wire cutting and/or machining 50 Ta 50 /Ti 80 Mo 20 Cutting raw material plate on the laminated composite plate, and obtaining the submicron structure with fresh surface (without dirt or surface scale) by mechanically grinding and ultrasonically cleaning the raw material plateZr (b) of 50 Ta 50 /Ti 80 Mo 20 A layered composite board;
(6) 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 (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: first, 120 pieces of Zr with submicron structure 50 Ta 50 /Ti 80 Mo 20 The layered composite plates were stacked, followed by two pieces of Zr in contact with the upper and lower iron plates of the second clad 50 Ta 50 /Ti 80 Mo 20 The surface of the layered composite board is coated with a glass lubricant for lubrication, and the well-stacked Zr is added 50 Ta 50 /Ti 80 Mo 20 The 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 2 Pa), and finally the square hole is sealed by adopting high-temperature vacuum sealing mud to obtain a second sheath plate blank;
(7) heating the second sheathing 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; in the extrusion process, the second sheathing plate blank is heated and insulated by an electric induction heater arranged in a bushing of an extrusion cylinder, the extrusion temperature is controlled at 550 ℃, and the extrusion ratio is 0.5;
(8) heating the extruded second sheathing board blank in a box-type resistance furnace at 650 ℃, and keeping the temperature for 30min; 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%;
(9) 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 at 675 ℃ for 30min to obtain Zr 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 Radical (Zr) 50 Ta 50 /Ti 80 Mo 20 ) A composite material.
(3) Alloy detection
Zr analysis by high-energy X-ray synchrotron radiation (HE-SXRD) 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 Radical (Zr) 50 Ta 50 /Ti 80 Mo 20 ) 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 0.4mm 2 At a wavelength of
Figure BDA0003065361170000131
FIG. 9 shows Zr in this example 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 High 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 Zr 50 Ta 50 /Ti 80 Mo 20 The composite material exhibits a unitary BCC structure as a whole.
Zr observation by FEI Nova Nano 450 field emission scanning electron microscope 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 Radical (Zr) 50 Ta 50 /Ti 80 Mo 20 ) 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 example 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 Scanning electron microscope photograph of the cross section of the base composite material. As can be seen, zr 50 Ta 50 /Ti 80 Mo 20 The composite material consists of Zr 50 Ta 50 Nanosheets (bright bands in the figure) and Ti 80 Mo 20 The matrix (dark areas in the figure) constitutes, presenting a typical layered composite structure. Wherein, zr 50 Ta 50 The average thickness of the nano-sheet is 93nm 50 Ta 50 Nanosheets being in Zr 50 Ta 50 /Ti 80 Mo 20 The composite material accounts for 22% of the volume fraction. In addition, it can be seen that Zr 50 Ta 50 Nanosheet and Ti 80 Mo 20 Absence at the interface of the substrateIn any adverse reactions such as eutectic or precipitation, a good metallurgical bond is formed.
For Zr on an Instron-8801 type tensile tester 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 Radical (Zr) 50 Ta 50 /Ti 80 Mo 20 ) The composite was subjected to a room temperature tensile test using tensile specimens along the Zr 50 Ta 50 /Ti 80 Mo 20 The 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 -3 s -1 . FIG. 11 shows Zr in this example 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 Stress-strain curve of the base composite during stretching. It can be seen that Zr 50 Ta 50 /Ti 80 Mo 20 The 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 Zr 50 Ta 50 /Ti 80 Mo 20 The 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 example 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 The 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 in this example 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 The performance ratio of the matrix composite material to the existing beta titanium alloy is 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 structure 50 Ta 50 Nanosheet reinforced Ti 80 Mo 20 The 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. a preparation method of a Zr-Ta nanosheet reinforced Ti-Mo based composite material is characterized by comprising the following steps:
    a) Alternately stacking Zr-Ta plates and Ti-Mo plates in the order of Ti-Mo/Zr-Ta/Ti-Mo/Zr-Ta … … Ti-Mo/Zr-Ta/Ti-Mo, and totally stacking 21 layers, wherein the Zr-Ta plates are Zr-Ta plates with Ta content of 30-50% by mass and size of (100-140 mm) x (50-70 mm) x (0.3-0.5 mm), the Ti-Mo plates are Ti-Mo plates with Mo content of 10-20% by mass and size of (100-140 mm) x (50-70 mm) x (1.7-1.5 mm),
    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 the heat for 20-30 min, and preheating before finishing 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 through a reserved square hole of the sheath to a vacuum degree range of 1-2 Pa, 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, and preserving heat for 10-30 min to finish 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 at 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 ℃ 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:
    the step B) of heating the sheathed plate blank to 600-700 ℃ and keeping the temperature for 20-30 min is carried out 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.
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