CN115305424A - Definite orientation ultrafine crystal pure titanium and preparation method thereof - Google Patents
Definite orientation ultrafine crystal pure titanium and preparation method thereof Download PDFInfo
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- CN115305424A CN115305424A CN202210806933.4A CN202210806933A CN115305424A CN 115305424 A CN115305424 A CN 115305424A CN 202210806933 A CN202210806933 A CN 202210806933A CN 115305424 A CN115305424 A CN 115305424A
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- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L27/00—Materials for grafts or prostheses or for coating grafts or prostheses
- A61L27/02—Inorganic materials
- A61L27/04—Metals or alloys
- A61L27/06—Titanium or titanium alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/12—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding
- B23K20/122—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding
- B23K20/1245—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating the heat being generated by friction; Friction welding using a non-consumable tool, e.g. friction stir welding characterised by the apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K20/00—Non-electric welding by applying impact or other pressure, with or without the application of heat, e.g. cladding or plating
- B23K20/26—Auxiliary equipment
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0081—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/08—Non-ferrous metals or alloys
- B23K2103/14—Titanium or alloys thereof
Abstract
The invention provides definite-orientation ultrafine-grained pure titanium, which belongs to the technical field of advanced structural materials, wherein the grain size of the ultrafine-grained pure titanium is 0.2-3 mu m, the average size of the ultrafine-grained pure titanium is 0.9 mu m, and the crystal orientations of the ultrafine-grained pure titanium are consistent and are all [0001] orientations. The pure titanium has an ultrafine crystal structure, and the ultrafine crystal is expressed as single orientation, has higher strength and plasticity, and can be used for biological implants and medical appliance structures. The invention also provides a preparation method of the definite orientation ultrafine crystal pure titanium.
Description
Technical Field
The invention belongs to the technical field of advanced structural materials, and particularly relates to definite-orientation ultrafine-grained pure titanium and a preparation method thereof.
Background
Pure titanium is one of important biomedical materials, and has excellent biocompatibility and resistance to corrosion of body fluid environment. Compared with titanium alloy, the titanium alloy is a pure metal material, and has no side effect on human body caused by toxic metal ions such as V, al, cr, co and the like, and no high cost caused by alloy elements such as Nb, ta, mo and the like. The existing pure titanium is forced to be in the cause of strength, and the medical application of the pure titanium is greatly limited. In order to solve the problem of low strength of the existing pure titanium, the structure of ultrafine crystal pure titanium is imperative.
Through the development of several generations of materials, the existing superfine crystal material preparation mostly adopts a severe plastic deformation mode, including channel rotating extrusion, rolling, forging and pressing and the like. However, in the case of titanium metal which is difficult to deform, the orientation of the crystal grains of an ultra-fine crystal structure having a severe plastic deformation structure is not easily controlled, and the processing is also difficult.
Disclosure of Invention
In order to solve the problem that the grain size and the grain orientation of the existing pure titanium are difficult to control, the invention provides the definite orientation ultrafine grain pure titanium, wherein the pure titanium has an ultrafine grain structure, and the ultrafine grain is expressed as single orientation.
The invention also provides a preparation method of the definite orientation ultrafine crystal pure titanium.
The invention is realized by the following technical scheme:
the grain size of the ultrafine grain pure titanium is 0.2-3 mu m, the average size is 0.9 mu m, and the crystal orientations of the ultrafine grain pure titanium are consistent and are all [0001 ].
Based on the same inventive concept, the application also provides the application of the definite-orientation ultrafine-grained pure titanium in preparing biomedical materials.
Based on the same inventive concept, the application also provides a preparation method of the definite orientation ultrafine grain pure titanium, which comprises the following steps:
carrying out heat treatment on the initial pure titanium plate to obtain a pure titanium plate with uniform tissue;
polishing the pure titanium plate with uniform tissue to obtain a smooth pure titanium plate;
and carrying out linear friction welding treatment on the smooth pure titanium plate, and then carrying out water cooling treatment to obtain the definite-orientation ultrafine-grained pure titanium.
Further, the heat treatment of the initial pure titanium plate to obtain a pure titanium plate with a uniform tissue specifically includes:
and (3) carrying out heat treatment on the initial pure titanium plate, wherein the heat treatment temperature is 500-600 ℃, the heat treatment time is 2-6 h, and air cooling is carried out after the heat treatment is finished to obtain the pure titanium plate with uniform tissue.
Further, the polishing treatment is performed on the pure titanium plate with the uniform tissue to obtain a smooth pure titanium plate, and the method specifically comprises the following steps:
and polishing the pure titanium plate with uniform tissue, wherein the polishing mode is mechanical polishing, and after the mechanical polishing is finished, the surface oil stain is removed by ultrasonic vibration cleaning to obtain the smooth pure titanium plate.
Further, the step of performing linear friction welding treatment on the smooth pure titanium plate and then performing water cooling treatment to obtain the definite-orientation ultrafine-grained pure titanium specifically comprises the following steps:
and performing linear friction welding treatment on the two smooth pure titanium plates, wherein the upsetting pressure of the linear friction welding treatment is 20-100 MPa, the welding frequency is 10-200 Hz, and the welding time is 2-8 s, and then performing water cooling treatment to obtain the oriented ultrafine-grained pure titanium.
Further, the post-water cooling treatment is carried out to obtain the definite orientation ultrafine crystal pure titanium, which specifically comprises the following steps:
and after the linear friction welding treatment is finished, performing water cooling treatment on the linear friction welding treatment part by using an ice-water mixture as a cooling liquid, wherein the pure titanium of the linear friction welding treatment part is the definite-orientation ultrafine-grained pure titanium.
Based on the same inventive concept, the application also provides the application of the preparation method of the definite orientation ultrafine crystal pure titanium in the preparation of biomedical materials.
One or more technical solutions in the embodiments of the present invention have at least the following technical effects or advantages:
1. the definite orientation ultrafine crystal pure titanium has an ultrafine crystal structure, and the ultrafine crystal is expressed as single orientation [0001], so that a sliding system is easy to start in the direction, the improvement of the plasticity of the pure titanium is facilitated, the ultrafine crystal structure endows the pure titanium with higher strength, the pure titanium can be used as a biomedical material, and the application range of the pure titanium in the field of medical materials is greatly expanded.
2. The invention relates to a preparation method of definite orientation ultrafine crystal pure titanium, which adopts linear friction welding to process pure titanium plates, one pure titanium plate does linear reciprocating motion relative to the other pure titanium plate along the direction of a splicing line at a specific welding frequency under the action of welding pressure, and the two titanium plates are welded into a whole through mutual diffusion and recrystallization under the combined action of friction heating and top forging pressure, so that an ultrafine crystal structure is obtained at a welding position, the problem that the ultrafine crystal structure is obtained from a coarse crystal structure of a pure titanium material is effectively solved, the obtained ultrafine crystal structure is expressed as a single specific orientation, and the problems of synchronously realizing grain refinement and crystal orientation regulation in pure titanium are effectively solved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on the drawings without creative efforts.
FIG. 1 is an electron back-scattered diffraction (EBSD) pattern of oriented ultra-fine grained pure titanium prepared according to an embodiment of the present invention;
FIG. 2 is an Electron Back Scattering Diffraction (EBSD) chart of the oriented ultra-fine grained pure titanium prepared in example 2 of the present invention;
FIG. 3 is a 50-fold enlarged view of the middle portion of FIG. 3 in accordance with the present invention;
FIG. 4 shows the preparation of ultra-fine grain titanium with definite orientation prepared by the embodiment of the present invention
A polar diagram;
FIG. 5 is a statistical graph of the grain size of the ultra-fine grain titanium prepared according to the present invention.
Detailed Description
The present invention will be described in detail below with reference to specific embodiments and examples, and the advantages and various effects of the present invention will be more clearly apparent therefrom. It will be understood by those skilled in the art that these specific embodiments and examples are for the purpose of illustrating the invention and are not to be construed as limiting the invention.
Throughout the specification, unless otherwise specifically noted, terms used herein should be understood as having meanings as commonly used in the art. Accordingly, unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. If there is a conflict, the present specification will control.
Unless otherwise specifically indicated, various raw materials, reagents, instruments, equipment and the like used in the present invention may be commercially available or may be prepared by existing methods.
The overall idea of the invention is as follows:
at present, the existing superfine crystal material preparation mostly adopts a severe plastic deformation mode, including channel rotating extrusion, rolling, forging and pressing and the like. However, in the case of titanium metal which is difficult to deform, the orientation of the crystal grains of an ultra-fine crystal structure having a severe plastic deformation structure is not easily controlled, and the processing is also difficult. In the application, a treatment mode of linear friction welding is creatively adopted, so that not only is grain refinement realized in polycrystalline pure titanium, but also single crystal orientation is synchronously regulated and controlled.
Specifically, the grain size of the ultrafine grain pure titanium is 0.2-3 microns, the average size of the ultrafine grain pure titanium is 0.9 microns, and the crystal orientations of the ultrafine grain pure titanium are consistent and are all [0001] orientations.
Based on the same inventive concept, the application also provides the application of the definite orientation ultrafine crystal pure titanium in preparing biomedical materials.
Based on the same inventive concept, the application also provides a preparation method of the definite orientation ultrafine grain pure titanium, which comprises the following steps:
carrying out heat treatment on the initial pure titanium plate to obtain a pure titanium plate with uniform tissue;
polishing the pure titanium plate with uniform tissue to obtain a smooth pure titanium plate;
and carrying out linear friction welding treatment on the smooth pure titanium plate, and then carrying out water cooling treatment to obtain the definite-orientation ultrafine-grained pure titanium.
In the application, the initial pure titanium plate adopts TA2, and the technical standard accords with GB/T3620.1-2007.
Further, the heat treatment is performed on the initial pure titanium plate to obtain a pure titanium plate with uniform coarse-grain structure, and the method specifically comprises the following steps:
and (3) carrying out heat treatment on the initial pure titanium plate, wherein the heat treatment temperature is 500-600 ℃, the heat treatment time is 2-6 h, and air cooling is carried out after the heat treatment is finished to obtain the pure titanium plate with uniform tissue.
Further, the polishing treatment is performed on the pure titanium plate with the uniform tissue to obtain a smooth pure titanium plate, and the method specifically comprises the following steps:
and polishing the pure titanium plate with uniform tissue, wherein the polishing mode is mechanical polishing, and after the mechanical polishing is finished, the surface oil stain is removed by ultrasonic vibration cleaning to obtain the smooth pure titanium plate.
In this application, the polishing process is intended to remove scratches on the surface of the pure titanium plate.
Further, the step of performing linear friction welding treatment on the smooth pure titanium plate and then performing water cooling treatment to obtain the definite-orientation ultrafine-grained pure titanium specifically comprises the following steps:
and performing linear friction welding treatment on the two smooth pure titanium plates, wherein the upsetting pressure of the linear friction welding treatment is 20-100 MPa, the welding frequency is 10-200 Hz, and the welding time is 2-8 s, and then performing water cooling treatment to obtain the oriented ultrafine-grained pure titanium.
In the application, the upsetting pressure of the linear friction welding treatment is 20-100 MPa, the welding frequency is 10-200 Hz, and the welding time is 2-8 s.
The method is favorable for forming the fixed-orientation ultrafine crystal structure at the welding joint by adopting linear friction welding treatment, the heading pressure and the welding frequency are lower than the range, the crystal grains are difficult to be oriented consistently, and the crystal grains are easy to grow up above the range.
Further, the post-water cooling treatment is carried out to obtain the definite orientation ultrafine crystal pure titanium, which specifically comprises the following steps:
and after the linear friction welding treatment is finished, performing water cooling treatment on the linear friction welding treatment part by using an ice-water mixture as a cooling liquid, wherein the pure titanium of the linear friction welding treatment part is the definite-orientation ultrafine-grained pure titanium.
The application relates to two times of cooling, wherein the first time of cooling is air cooling, so that the homogenization of coarse crystals of the structure is fully ensured; and an ice-water mixture is adopted for secondary cooling, so that the welding temperature is quickly reduced, the existence of ultrafine crystals is ensured, and the growth of the crystal grains is prevented.
Based on the same inventive concept, the application also provides the application of the preparation method of the definite orientation ultrafine grain pure titanium in the preparation of biomedical materials.
The present invention will be described in detail with reference to the following examples and experimental data.
Example 1
The embodiment provides a preparation method of definite-orientation ultrafine-grained pure titanium, which comprises the following specific preparation steps:
step 1: carrying out heat treatment on the initial pure titanium plate to obtain a uniform coarse crystal structure, wherein the grain size is 47 mu m;
selecting a pure titanium plate with a uniform structure and a thickness of 1mm, wherein the heat treatment temperature is 600 ℃, the heat treatment time is 3 hours, and the cooling mode is air cooling;
step 2: polishing the titanium plate prepared in the step 1 to obtain a pure titanium plate with a smooth surface;
polishing the titanium with the coarse-grain structure by adopting mechanical polishing, and finely polishing by using fine wool fabric to remove surface scratches; and ultrasonic vibration cleaning to remove oil stains on the surface.
And step 3: performing linear friction welding treatment on the smooth pure titanium plate prepared in the step 2 to obtain single-orientation ultrafine-grained pure titanium;
and (3) processing the smooth titanium plate by adopting linear friction welding, wherein the upsetting pressure is 50MPa, the welding frequency is 50Hz, and the welding time is 8s.
And 4, step 4: step 3, performing water cooling treatment on the titanium plate subjected to the linear friction welding treatment;
an ice-water mixture was used as the cooling liquid.
As shown in FIG. 1, two sides in FIG. 1 show coarse-grain structure, which is a pure titanium plate with uniform initial structure; the middle is an ultra-fine grain structure and is a linear friction welding joint.
Example 2
The embodiment provides a preparation method of definite-orientation ultrafine-grained pure titanium, which comprises the following specific preparation steps:
step 1: carrying out heat treatment on the initial pure titanium plate to obtain a uniform coarse crystal structure, wherein the grain size is about 32 mu m;
selecting a pure titanium plate with a uniform structure and a thickness of 1mm, wherein the heat treatment temperature is 550 ℃, the heat treatment time is 3 hours, and the cooling mode is air cooling;
step 2: polishing the titanium plate prepared in the step 1 to obtain a pure titanium plate with a smooth surface;
polishing the titanium with the coarse-grain structure by adopting mechanical polishing, and finely polishing through fine wool fabric to remove surface scratches; and ultrasonic vibration cleaning to remove oil stains on the surface.
And step 3: performing linear friction welding treatment on the smooth pure titanium plate prepared in the step 2 to obtain single-orientation ultrafine-grained pure titanium;
and (3) processing the smooth titanium plate by adopting linear friction welding, wherein the upsetting pressure is 50MPa, the welding frequency is 50Hz, and the welding time is 4s.
And 4, step 4: step 3, performing water cooling treatment on the titanium plate subjected to the linear friction welding treatment;
an ice-water mixture was used as the cooling liquid.
As shown in fig. 2, both sides of fig. 2 show coarse-grained structures, which are pure titanium plates with uniform initial structures; the middle of the welding rod is of an ultra-fine grain structure and is a linear friction welding joint.
As shown in fig. 3, fig. 3 is an enlarged representation of the intermediate structure of the welded joint of fig. 2 as an equiaxed ultrafine grain structure;
as shown in fig. 4, fig. 4 is a polar view of the intermediate structure of the welded joint in fig. 2, with the crystal orientation collectively represented as [0001] orientation;
as shown in fig. 5, fig. 5 is a statistical graph of the grain size of the intermediate structure of the welded joint in fig. 2, and the average size of the crystal is 0.9 μm, such an ultra-fine grain structure can greatly improve the strength of the pure titanium.
By observing the microstructure and the grain size of FIGS. 2 to 5, it was found that the joint bonding portion of the present invention was changed from an initial grain size of about 32 μm to a definite orientation ultra-fine grain having a grain size of about 0.9 μm by the linear friction welding process. Meanwhile, the pole figure is observed, and the ultra-fine grain structure of the joint part is uniformly expressed as the [0001] orientation.
Finally, it should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (8)
1. The fixed orientation superfine crystal pure titanium is characterized in that the grain size of the superfine crystal pure titanium is 0.2-3 mu m, the average size is 0.9 mu m, and the crystal orientations of the superfine crystal pure titanium are consistent and are all [0001] orientation.
2. Use of the ultra-fine grain oriented pure titanium according to claim 1 for the preparation of biomedical materials.
3. A method for preparing the oriented ultrafine grained pure titanium according to claim 1, wherein the method comprises:
carrying out heat treatment on the initial pure titanium plate to obtain a pure titanium plate with uniform tissue;
polishing the pure titanium plate with uniform tissue to obtain a smooth pure titanium plate;
and carrying out linear friction welding treatment on the smooth pure titanium plate, and then carrying out water cooling treatment to obtain the definite-orientation ultrafine-grained pure titanium.
4. The method for preparing ultra-fine grain pure titanium with definite orientation according to claim 3, wherein the step of heat-treating the initial pure titanium plate to obtain the pure titanium plate with uniform tissue comprises:
and (3) carrying out heat treatment on the initial pure titanium plate, wherein the heat treatment temperature is 500-600 ℃, the heat treatment time is 2-6 h, and air cooling is carried out after the heat treatment is finished to obtain the pure titanium plate with uniform tissue.
5. The method as claimed in claim 3, wherein said polishing said pure titanium plate with uniform structure to obtain a smooth pure titanium plate comprises:
and polishing the pure titanium plate with uniform tissue, wherein the polishing mode is mechanical polishing, and after the mechanical polishing is finished, the surface oil stain is removed by ultrasonic vibration cleaning to obtain the smooth pure titanium plate.
6. The method for preparing the definite orientation ultrafine grain pure titanium according to claim 3, wherein the step of subjecting the smooth pure titanium plate to linear friction welding treatment and then to water cooling treatment to obtain the definite orientation ultrafine grain pure titanium specifically comprises:
and performing linear friction welding treatment on the two smooth pure titanium plates, wherein the upsetting pressure of the linear friction welding treatment is 20-100 MPa, the welding frequency is 10-200 Hz, and the welding time is 2-8 s, and then performing water cooling treatment to obtain the oriented ultrafine crystal pure titanium.
7. The method for preparing oriented ultrafine grained pure titanium according to claim 6, wherein said post-water cooling treatment is performed to obtain oriented ultrafine grained pure titanium, and the method comprises:
and after the linear friction welding treatment is finished, water cooling treatment is carried out on the linear friction welding treatment part by taking an ice water mixture as cooling liquid, and the pure titanium of the linear friction welding treatment part is the oriented ultrafine grained pure titanium.
8. Use of the method for producing the ultrafine grain oriented pure titanium according to claim 3 for producing biomedical materials.
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