CN114411074B - Preparation method of multilayer biphase trans-scale structure pure titanium - Google Patents
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- CN114411074B CN114411074B CN202111522266.9A CN202111522266A CN114411074B CN 114411074 B CN114411074 B CN 114411074B CN 202111522266 A CN202111522266 A CN 202111522266A CN 114411074 B CN114411074 B CN 114411074B
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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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- 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
- C21D1/00—General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
- C21D1/26—Methods of annealing
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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
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0221—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the working steps
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- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
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- 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
- C22F3/00—Changing the physical structure of non-ferrous metals or alloys by special physical methods, e.g. treatment with neutrons
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Abstract
The invention discloses a preparation method of pure titanium with a multilayer two-phase trans-scale structure, wherein the multilayer two-phase trans-scale structure is formed by nanocrystalline alpha titanium-fine crystalline alpha titanium-coarse crystalline beta titanium. The preparation method of the multilayer biphase trans-scale structure pure titanium comprises the following steps: step 1: carrying out multi-pass rolling on the titanium plate at room temperature to obtain nanocrystalline alpha pure titanium; step 2: annealing the recovery of the nanocrystalline alpha pure titanium obtained in the step 1; and step 3: and (3) carrying out etching heat treatment on the nanocrystalline alpha pure titanium obtained in the step (2) by using a high-energy electron beam in a vacuum environment to obtain a multi-layer double-phase nanocrystalline alpha titanium-fine crystalline alpha titanium-coarse crystalline beta titanium cross-scale structure. The invention solves the problem of obtaining the trans-scale uneven structure pure titanium from the nanocrystalline pure titanium, the obtained multilayer biphase trans-scale structure pure titanium can be used as a biological implant bearing structure material, the preparation process is simple and efficient, and the large-scale production can be realized. In addition, the preparation method can also be used in the fields of nanocrystalline material surface modification and the like.
Description
Technical Field
The invention relates to the technical field of metal material processing and preparation or medical surgery implant, in particular to a preparation method of multilayer biphase trans-scale structure pure titanium.
Background
Through the development of several generations of materials, the mechanical properties of the nanocrystalline metal material are improved dramatically, and the mechanical properties of the material, such as strength, fatigue damage resistance, frictional wear resistance and the like, are improved greatly to better meet the engineering requirements. However, practical engineering applications of nanocrystalline metal materials still have significant limitations, including their disadvantages of low ductility, low damage tolerance, low thermal stability, etc. Therefore, material scientists have focused on developing new structural materials that combine the advantages of both traditional and nanocrystalline metallic materials, and the cross-scale heterogeneous (multiphase or multilayer) structures are currently the most promising design concept for structural materials.
The design ideas of the trans-scale uneven structure mainly comprise two kinds, one is to prepare a nanocrystalline layer on a coarse-grain substrate or add a surface layer of another phase on a single-phase substrate, and the idea belongs to the surface mechanical nanocrystallization and the prepared gradient structure thereof; and secondly, obtaining nanocrystalline metal firstly, and then carrying out heat treatment on the surface or the inside of the nanocrystalline metal to obtain a coarse crystal part. Both of these concepts result in a cross-scale non-uniform structural material with greatly improved surface or overall properties. However, the two approaches described above are difficult to achieve with difficult-to-deform metals such as titanium, nitinol, and many large structural components. In the face of the problem, a new method of a multilayer two-phase cross-scale structure, which is simple, efficient and capable of industrial production, is urgently needed to be developed on the basis of the existing method principle.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a preparation method of multilayer dual-phase trans-scale structure pure titanium, which adopts the technical means of preparing the multilayer dual-phase trans-scale structure pure titanium by using nanocrystalline titanium, solves the problem of preparing the multilayer dual-phase trans-scale structure pure titanium by using nanocrystalline bulk pure titanium, and solves the problems mentioned in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the multilayer dual-phase trans-scale structure pure titanium is composed of nanocrystalline alpha titanium-fine crystalline alpha titanium-coarse crystalline beta titanium.
A preparation method of multilayer biphase trans-scale structure pure titanium comprises the following steps:
preferably, the cumulative strain of the multi-pass room temperature rolling in the step 1 is more than or equal to 80%, and the strain of each pass is less than or equal to 10%.
Preferably, the grain size of the nanocrystalline alpha titanium in the step 1 is 80nm to 200 nm.
Preferably, the annealing for recoverability in the step 2 specifically comprises: heating from room temperature to 200-400 ℃ at a heating rate of 8-10 ℃/min, preserving heat for 10min, then reducing the temperature to the ambient temperature at a cooling rate of 3-5 ℃/min, and cooling.
Preferably, the vacuum degree during the etching heat treatment in the step 3 is not lower than 5 Pa.
Preferably, the current of the high-energy electron beam in the step 3 is 2 mA-10 mA, and the feeding speed of the electron gun is 5 m/min-20 m/min.
The process principle for obtaining the coarse-grain beta titanium on the nano-crystal alpha titanium substrate provided by the invention is as follows: when the electron beam is fed and moved to the next area, the melted sample in the previous area is quickly dissipated due to the small heat in the area, and a large amount of needle-shaped beta titanium crystal grains are generated when the sample is reduced to the temperature of a phase change point due to quick cooling.
The process principle of the multilayer trans-scale structure retention is as follows: the heat input is reasonably controlled to ensure that the heat of etching heat treatment is locally effective and quickly dissipated, and three areas, namely a heat treatment core area, a heat affected area and a recovery matrix, are formed. Rapidly heating the heat treatment core area until the heat treatment core area is melted, and rapidly cooling to form coarse-grain beta titanium; the heat affected zone causes thermally activated static recrystallization due to heat transfer effect, and because the temperature of the heat affected zone is lower than the phase transition temperature, grains in the heat affected zone cannot be coarsened quickly to form fine-grain alpha titanium, and the thickness of the heat affected zone is determined by heat input quantity, particularly by excitation current and electron gun feeding speed; the temperature of the matrix region is lower when the heat is transferred to a more distant region, and only the static recovery of the matrix can be realized, and the static recrystallization is not enough, so that the matrix nanocrystalline alpha titanium still remains. The step 2 of annealing the recovery of the nanocrystalline alpha titanium is to reduce the dislocation density and distortion energy of the matrix, so that the matrix is less prone to recrystallization, the heat input during etching heat treatment is easier, and the large-area recrystallization and local abnormal grain growth of the matrix are prevented, which is a necessary condition for forming a cross-scale multiphase structure of the nanocrystalline alpha titanium-fine crystalline alpha titanium-coarse crystalline beta titanium.
The invention has the beneficial effects that:
1) the preparation method of the multilayer double-phase trans-scale structure pure titanium provided by the invention obtains the multilayer double-phase trans-scale structure of nano-crystalline alpha titanium-fine crystalline alpha titanium-coarse crystalline beta titanium, solves the problem of obtaining the multilayer double-phase trans-scale pure titanium by the nano-crystalline pure titanium, and provides a potential solution for the trans-scale structure design of other superfine crystalline/nano-crystalline difficult-to-deform metals;
2) the preparation method of the multilayer double-phase cross-scale structure pure titanium provided by the invention is different from the traditional thermal treatment process, and the high-energy electron beam can be used for processing a complex component without damaging the strength advantage of the component.
3) The preparation method of the multilayer biphase trans-scale structure pure titanium provided by the invention has the advantages of simple preparation process and high efficiency, and can be used in the fields of nanocrystalline material surface modification and the like.
Drawings
FIG. 1 is a graph showing the hardness distribution of each layer of pure titanium in a multi-layer two-phase trans-scale structure prepared in examples 1 and 2 of the present invention;
FIG. 2 is an optical picture of pure titanium with a non-uniform structure prepared in examples 1-4 of the present invention;
FIG. 3 is a high power optical picture of pure titanium side of the multi-layer dual-phase trans-scale structure obtained in example 1 of the present invention;
FIG. 4 is a Transmission Electron Microscope (TEM) image of the multi-layer dual-phase trans-scale structure pure titanium nanocrystalline alpha titanium obtained in example 1 of the present invention;
FIG. 5 is a high power optical image of the multi-layer dual-phase trans-scale structure pure titanium macrocrystalline beta titanium obtained in example 1 of the present invention;
FIG. 6 is a high power optical picture of pure titanium side of the multi-layer dual-phase trans-scale structure obtained in example 2 of the present invention;
FIG. 7 is a high power optical picture of a side of pure titanium with a non-uniform structure obtained in example 3 of the present invention;
FIG. 8 is a high power optical image of a side of pure titanium with a non-uniform structure obtained in example 4 of the present invention;
FIG. 9 is a schematic diagram of the application of the preparation method of the present invention to etching of nanocrystalline titanium.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The raw material is TA2, and the component standard conforms to GB/T3620.1-2007.
Example 1
The preparation method of the multilayer biphase cross-scale structure pure titanium comprises the following specific steps:
a pure titanium plate with a thickness of 8mm is used as a starting material, and the starting material is cut into a length, a width and a height which are 40 mm multiplied by 12 mm multiplied by 8mm 3 The pure titanium plate of (2);
the roller spacing of the rolling mill is adjusted to be 8mm, and the rotating speed is equal to 20 mm/s.
Adjusting the distance between the rollers to reduce by 0.1mm, feeding the sample into the rollers to finish 1-pass rolling, converting the feeding direction of the plate, and performing second-pass rolling on the plate.
The above rolling process was repeated until a pure titanium plate having a thickness of 1mm was obtained.
The microstructure of the room temperature rolled sample consisted of elongated lath-like alpha grains with an average grain size of about 150 nm.
and (3) performing recovery annealing on the pure titanium plate with the thickness of 1mm obtained in the step (1) in a vacuum tube furnace.
And (3) putting the sample into a vacuum tube furnace, heating the sample from room temperature to 400 ℃ at a heating rate of 10 ℃/min, preserving the heat for 10min, then cooling the sample to 50 ℃ at a cooling rate of 5 ℃/min, cooling, inflating the vacuum tube furnace, and taking out the recovered nanocrystalline alpha titanium.
and (3) placing the pure titanium plate obtained in the step (2) in a working chamber of an electron beam welding machine, and starting a vacuum pump to pump vacuum.
And setting parameters of an electron gun after the vacuum degree meets the requirement, wherein the electron beam and the sample form 90 degrees, the excitation current is 5mA, the moving mode of the electron gun is set to be single linear movement, and the moving speed is 10 m/min.
The moving stroke direction of the electron gun is parallel to the rolling direction of the rolled plate, and the total stroke is slightly smaller than the length of the rolled plate obtained in the steps 1 and 2.
And after the etching heat treatment is finished and the cooling is carried out, the multi-layer double-phase cross-scale structure formed by the nano-crystalline alpha titanium-fine crystalline alpha titanium-coarse crystalline beta titanium is obtained.
The solid circle connecting line in fig. 1 is a graph of the hardness distribution rule of each layer of the multilayer dual-phase trans-scale structure pure titanium prepared by the steps, and it can be seen that the hardness value of the matrix nanocrystalline alpha titanium is still kept at 280HV and is close to the hardness (292HV) of a sample subjected to room temperature rolling and annealing. The hardness value rapidly decreases from 280HV to around 180HV as the center of the etching heat treatment is approached, and the width of the transition zone is about 180 μm. The hardness value is slowly raised to 200HV after the lowest point, about 250 μm later, the total width of the heat affected zone of the etching heat treatment is about 3mm, and the gold phase diagram of example 1 in FIG. 2 corresponds to the hardness diagram of the solid circle connecting line.
Fig. 3 is a high power optical picture of one side of the multilayer dual-phase trans-scale structure pure titanium prepared by the above steps, and it can be seen that the metallographic phase of the nanocrystalline alpha titanium (fig. 4 electron microscopic picture) is a slender fibrous structure, the grains are changed into equiaxed fine crystalline alpha titanium near the etching heat treatment core area, and coarse crystalline beta titanium is in the etching heat treatment center (fig. 5 high power optical picture).
The multi-layer two-phase cross-scale structure prepared in example 1 shows that only the matrix nanocrystalline alpha titanium is recovered, the heat input in the etching heat treatment process does not recrystallize the whole sample, the etching heat treatment central area is violently and dynamically recrystallized even is close to a molten state due to sufficient heat input, and the etching heat treatment central area is changed into coarse-grained acicular beta titanium through rapid cooling.
Example 2
In the step 3, the excitation current of the electron beam etching heat treatment is 10mA, and the recovery annealing comprises the following steps: putting the sample into a vacuum tube furnace, heating the sample from room temperature to 300 ℃ at a heating rate of 8 ℃/min, preserving the heat for 10min, then reducing the temperature to the ambient temperature (below 50 ℃) at a cooling rate of 5 ℃/min, cooling, inflating the vacuum tube furnace, and taking out the recovered nanocrystalline alpha titanium. The remaining procedure was exactly the same as in example 1.
The hollow round connecting line in fig. 1 is a graph showing the hardness distribution rule of each layer of the multilayer dual-phase trans-scale structure pure titanium prepared in the above step example 2, and compared with example 1, the hardness value of the matrix nanocrystalline alpha titanium is reduced to about 260 HV. The hardness values varied similarly to example 1 as the center of the etching heat treatment approached, and unlike example 1, the total width of the heat affected zone of the etching heat treatment increased to about 4mm, and the gold phase diagram of example 2 in fig. 2 corresponded to the open circle-lined hardness diagram.
Compared with the example 1, the increase of the total width of the heat affected zone of the etching heat treatment and the reduction of the hardness of the matrix nano-crystalline alpha titanium indicate that the heat input in the example 2 is higher than that in the example 1, but the original microstructure of the matrix nano-crystalline alpha titanium can be still maintained under the parameters, as shown in fig. 6, which indicates the universality of the preparation method and the suitability for more working conditions.
Example 3
In the step 3, the exciting current of the electron beam etching heat treatment is 10mA, the moving speed of an electron gun is 2m/min, and the recovery annealing comprises the following steps: putting the sample into a vacuum tube furnace, heating the sample from room temperature to 200 ℃ at a heating rate of 10 ℃/min, preserving the heat for 10min, then reducing the temperature to below 50 ℃ at a cooling rate of 3 ℃/min, cooling, inflating the vacuum tube furnace, and taking out the recovered nanocrystalline alpha titanium. The rest of the procedure was exactly the same as in example 1.
As can be seen from fig. 7, unlike examples 1 and 2, the matrix nanocrystals of example 3 were not present and became completely fine-grained α titanium, which resulted in a decrease in the overall strength of the sample and failed to maintain the multi-layer dual-phase trans-scale structure of nanocrystalline α titanium-fine-grained α titanium-coarse-grained β titanium. This is because the electron gun moves too slowly and heat input is too high, which results in severe recrystallization of the whole sample and destruction of the matrix structure and strength of the sample.
Example 4
The excitation current of the electron beam etching heat treatment in step 3 was 20mA, the moving speed of the electron gun was 10m/min, and the rest of the steps were completely the same as in example 1.
As can be seen from fig. 8, unlike examples 1 and 2, the matrix nanocrystals of example 4 were not present and became completely coarse α titanium, which resulted in a significant decrease in the overall strength of the sample and failed to maintain the multi-layer dual-phase trans-scale structure of α titanium nanocrystals- β titanium nanocrystals.
Combining example 3 and example 4, too slow of electron gun movement or too large of excitation current (too much power) resulted in too much heat input, resulting in severe recrystallization of the entire sample and destruction of the matrix structure and strength of the sample.
Application example 1
Fig. 9 is an application schematic diagram of the preparation method of the invention for etching nanocrystalline titanium, the width depth and the geometric shape of the etching heat treatment region can be adjusted by adjusting parameters such as the excitation current and the moving speed, and for nanocrystalline titanium, the etching heat treatment can easily obtain a pseudo-topological structure with a complex geometric shape on the surface, and the structural advantage and the strength advantage of the nanocrystalline matrix are not lost, so that the preparation method is an efficient and convenient industrial means.
The preparation method of the multilayer dual-phase trans-scale structure pure titanium provided by the invention is not limited to the application in the technical field of metal material processing and preparation or medical surgical implants, and the application of the preparation method of the multilayer dual-phase trans-scale structure pure titanium provided by the invention in any field and industry belongs to the protection scope of the patent.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (3)
1. A preparation method of multilayer biphase trans-scale structure pure titanium is characterized by comprising the following steps: the method comprises the following steps:
step 1, carrying out multi-pass rolling on a titanium plate at room temperature to obtain nanocrystalline alpha pure titanium;
step 2, annealing the nanocrystalline alpha pure titanium plate obtained in the step 1 in a recovery manner;
step 3, carrying out etching heat treatment on the nanocrystalline alpha pure titanium obtained in the step 2 by using a high-energy electron beam in a vacuum environment to obtain a multi-layer double-phase nanocrystalline alpha titanium-fine crystalline alpha titanium-coarse crystalline beta titanium cross-scale structure;
the recovery annealing in the step 2 specifically comprises the following steps: heating from room temperature to 200-400 ℃ at a heating rate of 5-10 ℃/min, preserving heat for 5-30 min, then reducing the temperature to the ambient temperature at a cooling rate of 3-5 ℃/min, and cooling;
the vacuum degree during the etching heat treatment in the step 3 is not lower than 5 Pa;
in the step 3, the current of the high-energy electron beam is 2 mA-15 mA, and the feeding speed of the electron gun is 5 m/min-20 m/min.
2. The method for preparing pure titanium with a multi-layer dual-phase trans-scale structure according to claim 1, wherein the method comprises the following steps: the cumulative strain of the multi-pass room temperature rolling in the step 1 is more than or equal to 80 percent, and the strain of each pass is less than or equal to 10 percent.
3. The method for preparing pure titanium with a multi-layer dual-phase trans-scale structure according to claim 1, wherein the method comprises the following steps: the grain size of the nanocrystalline alpha titanium in the step 1 is 80 nm-200 nm.
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