CN110042335B - Treatment process for obtaining complete recrystallization structure of titanium-zirconium alloy with low zirconium content - Google Patents
Treatment process for obtaining complete recrystallization structure of titanium-zirconium alloy with low zirconium content Download PDFInfo
- Publication number
- CN110042335B CN110042335B CN201910290266.7A CN201910290266A CN110042335B CN 110042335 B CN110042335 B CN 110042335B CN 201910290266 A CN201910290266 A CN 201910290266A CN 110042335 B CN110042335 B CN 110042335B
- Authority
- CN
- China
- Prior art keywords
- titanium
- rolling
- zirconium alloy
- zirconium
- alloy
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
-
- 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
Abstract
The invention discloses a treatment process for obtaining a complete recrystallization structure of a titanium-zirconium alloy with low zirconium content. The method comprises the following steps: 1) selecting titanium-zirconium alloy with low zirconium content as a heat treatment material; 2) carrying out acid pickling corrosion on the titanium-zirconium alloy by using a high-concentration corrosive liquid to remove surface oxide skin, and then cleaning and drying by using a cleaning liquid; 3) hot rolling the dried alloy; 4) carrying out first heat treatment on the titanium-zirconium alloy subjected to hot rolling treatment; 5) carrying out warm rolling on the treated alloy; 6) carrying out secondary heat treatment on the titanium-zirconium alloy subjected to warm rolling treatment; 7) and cleaning and drying the treated titanium-zirconium alloy by using a cleaning solution. The treatment process for obtaining the titanium-zirconium alloy complete recrystallization structure provided by the invention is simple and easy to implement, and related equipment, medicines and the like are common and easy to obtain. The method can obtain fine grains in the titanium zirconium alloy to toughen the material, and meets the requirement of clinical application of dental implants.
Description
Technical Field
The invention relates to a treatment process for obtaining a fully recrystallized structure of a titanium-zirconium alloy, in particular to a treatment process for fully recrystallizing a titanium-zirconium alloy with low zirconium content (Zr percent is less than or equal to 20 percent).
Background
As a novel implant material, the titanium-zirconium alloy makes up the defects of the mechanical property of a pure titanium implant and the biocompatibility of a Ti6Al4V implant, and has wide application prospect in the field of oral implantation. However, after adding zirconium to pure titanium, solute atoms interact with grain boundaries and dislocations, pinning the grain boundaries and dislocations, and hindering the grain boundary migration and the slippage and climbing of dislocations, so that the nucleation and growth of recrystallization become difficult.
The common method for obtaining complete metal recrystallization is annealing after rolling, but because the titanium zirconium alloy is hard, if the titanium zirconium alloy is cold-rolled at room temperature, the reduction is small, and enough activation energy is difficult to store for later recrystallization in the rolling process; in the case of high-temperature rolling, although a large reduction can be ensured, the activation energy stored in the previous rolling is dissipated due to the high temperature. Therefore, it becomes necessary to explore a treatment process capable of obtaining a fully recrystallized structure of the titanium-zirconium alloy, refine grains to improve the comprehensive mechanical properties of the titanium-zirconium alloy, and meet clinical requirements.
Disclosure of Invention
The invention aims to provide a treatment process for obtaining a fully recrystallized structure of a titanium-zirconium alloy with low zirconium content.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the treatment process for the complete recrystallization of the low-zirconium-content titanium-zirconium alloy comprises the following steps:
1) selecting titanium-zirconium alloy with low zirconium content as a heat treatment material;
2) carrying out acid pickling corrosion on the titanium-zirconium alloy by using a high-concentration corrosive liquid to remove surface oxide skin, and then cleaning and drying by using a cleaning liquid;
3) hot rolling the dried alloy;
4) carrying out first heat treatment on the titanium-zirconium alloy subjected to hot rolling treatment;
5) carrying out warm rolling on the treated alloy;
6) carrying out secondary heat treatment on the titanium-zirconium alloy subjected to warm rolling treatment;
7) and cleaning and drying the treated titanium-zirconium alloy by using a cleaning solution.
The corrosive liquid obtained by acid cleaning is HF HNO3:H2The method comprises the following steps of O1: 3: 10, cleaning fluid is acetone solution, ultrasonic cleaning, heat treatment in a vacuum furnace is adopted for heat treatment below the transition temperature of α + β/α, heat preservation is carried out for 3min each time, the rolling gap is slowly reduced until the reduction rate is 50%, unidirectional rolling is adopted, the first heat treatment process is carried out for heat preservation for 36h at the temperature of 50 ℃ below the transition temperature of α + β/α, the warm rolling process is carried out for heat preservation for 3min each time at a lower temperature or at room temperature, the rolling gap is slowly reduced until the reduction rate is 50%, unidirectional rolling is adopted, the second heat treatment process is carried out for heat treatment in the vacuum furnace, heat preservation is carried out for a plurality of hours at the temperature of 50 ℃ below the transition temperature of α + β/α, and the weight percentage of the low-zirconium-content titanium-zirconium alloy is less than or equal to 20%.
The treatment process for obtaining the titanium-zirconium alloy complete recrystallization structure provided by the invention is simple and easy to implement, and related equipment, medicines and the like are common and easy to obtain. The method can obtain fine grains in the titanium zirconium alloy to toughen the material, and meets the requirement of clinical application of dental implants.
Drawings
FIG. 1 is a metallographic photograph showing the complete recrystallization of a strip of a titanium-zirconium alloy containing 12% zirconium according to example 1 of the present invention after two rolling and annealing processes;
FIG. 2 is a metallographic photograph showing incomplete recrystallization of a strip of a titanium-zirconium alloy having a zirconium content of 16% and an oxygen content of 0.2% in inventive example 2, after a single rolling and annealing for 36 hours;
FIG. 3 is a metallographic photograph showing complete recrystallization of a Ti-Zr alloy strip having 16% Zr content and 0.2% O content according to inventive example 2, after a combined process of rolling twice and annealing;
FIG. 4 is a stress-strain curve obtained by subjecting a sample, as a starting material, of a titanium-zirconium alloy having a zirconium content of 16% and an oxygen content of 0.2% after complete recrystallization to a tensile test after working in inventive example 2;
fig. 5 is a metallographic photograph showing the complete recrystallization obtained after the strip of a titanium-zirconium alloy containing 20% zirconium according to inventive example 3 was subjected to a process combining two rolling passes and annealing.
Detailed Description
The treatment process for the complete recrystallization of the low-zirconium-content titanium-zirconium alloy comprises the following steps:
1) selecting titanium-zirconium alloy with low zirconium content as a heat treatment material;
2) carrying out acid pickling corrosion on the titanium-zirconium alloy by using a high-concentration corrosive liquid to remove surface oxide skin, and then cleaning and drying by using a cleaning liquid;
3) hot rolling the dried alloy;
4) carrying out first heat treatment on the titanium-zirconium alloy subjected to hot rolling treatment;
5) carrying out warm rolling on the treated alloy;
6) carrying out secondary heat treatment on the titanium-zirconium alloy subjected to warm rolling treatment;
7) and cleaning and drying the treated titanium-zirconium alloy by using a cleaning solution.
The corrosive liquid obtained by acid cleaning is HF HNO3:H2O1: 3: 10, the cleaning solution is acetone solution, ultrasonic cleaning, the hot rolling process is that the temperature is maintained for 3min each time at the conversion temperature of α + β/α, the rolling gap is reduced slowly until the reduction rate is 50%, unidirectional rolling is adopted, and the first heat treatment process is that the rolling is carried out in one directionThe method comprises the steps of adopting a vacuum furnace for heat treatment, and keeping the temperature below the transformation temperature of α + β/α at 50 ℃ for 36h, wherein the warm rolling process comprises the steps of keeping the temperature for 3min at a lower temperature or room temperature each time, slowly reducing the rolling gap until the reduction rate is 50%, and adopting unidirectional rolling, the second heat treatment process comprises the step of adopting a vacuum furnace for heat treatment, keeping the temperature below the transformation temperature of α + β/α at 50 ℃ for a plurality of hours, and the weight percentage of the low-zirconium-content titanium-zirconium alloy is (Zr% is less than or equal to 20%).
The invention will be further illustrated with reference to specific embodiments:
example 1
The selected titanium zirconium alloy lath with low zirconium content accounts for 12 percent by weight, and instruments used in the complete recrystallization treatment process comprise a KQ-50B type ultrasonic cleaner, a box-type resistance furnace, a muffle furnace with a Nabo hot brick structure, an optical metallographic microscope and a rolling mill. Firstly, the volume ratio of HF to HNO for the titanium-zirconium alloy with the thickness of 12mm3:H2O is 1: 3: 10, carrying out acid pickling corrosion on the corrosive liquid to remove surface oxide skin, and then cleaning and drying the corrosive liquid by using an acetone solution; then, unidirectionally rolling the titanium-zirconium alloy with the thickness of 12mm to the thickness of 6mm at the temperature of 500 ℃, and then preserving heat for 36 hours at the temperature of 750 ℃; then, unidirectionally rolling the titanium-zirconium alloy with the thickness of 6mm to the thickness of 3mm at room temperature, and then preserving heat at 750 ℃ for 1 h; and finally, cleaning and drying the treated titanium-zirconium alloy by using an acetone solution. As shown in FIG. 1, the results of the test showed that a completely recrystallized structure with a clear boundary and a uniform crystal grain size was obtained.
Example 2
The selected titanium zirconium alloy lath with low zirconium content has the weight percentage of 16 percent of Zr and 0.3 percent of O, and instruments used in the complete recrystallization treatment process comprise a KQ-50B type ultrasonic cleaner, a box type resistance furnace, a muffle furnace with a Nabo hot brick structure, an optical metallographic microscope and a rolling mill. Firstly, the volume ratio of HF to HNO for the titanium-zirconium alloy with the thickness of 12mm3:H2O is 1: 3: 10, carrying out acid pickling corrosion on the corrosive liquid to remove surface oxide skin, and then cleaning and drying the corrosive liquid by using an acetone solution; then the titanium zirconium alloy with 12mm is unidirectionally rolled to 6mm at 650 ℃, and then is kept warm for 36 hours at 650 ℃, and the test result is shown in figure 2, wherein the grain boundary is not clear, and part of the titanium zirconium alloy is not sinteredA bar-shaped structure of the crystal; then, unidirectionally rolling the titanium-zirconium alloy with the thickness of 6mm to the thickness of 3mm at the temperature of 500 ℃, and then preserving heat for 36 hours at the temperature of 650 ℃; and finally, cleaning and drying the treated titanium-zirconium alloy by using an acetone solution. As shown in FIG. 3, the results of the test showed that a completely recrystallized structure with a clear boundary and a uniform crystal grain size was obtained. The material is used as a raw material, and a tensile test is carried out after the material is processed, and the obtained stress-strain curve is shown in fig. 4, the tensile strength of the material exceeds 800MPa, the elongation at break is close to 20 percent, and the material is expected to replace pure titanium and Ti6Al4V to become a new implant material.
Example 3
The selected titanium zirconium alloy lath with low zirconium content accounts for 20 percent by weight of Zr, and instruments used in the complete recrystallization treatment process comprise a KQ-50B type ultrasonic cleaner, a box-type resistance furnace, a muffle furnace with a Nabo hot brick structure, an optical metallographic microscope and a rolling mill. Firstly, the volume ratio of HF to HNO for the titanium-zirconium alloy with the thickness of 12mm3:H2O is 1: 3: 10, carrying out acid pickling corrosion on the corrosive liquid to remove surface oxide skin, and then cleaning and drying the corrosive liquid by using an acetone solution; then, unidirectionally rolling the titanium-zirconium alloy with the thickness of 12mm to the thickness of 6mm at the temperature of 650 ℃, and then preserving heat for 36 hours at the temperature of 700 ℃; then, unidirectionally rolling the titanium-zirconium alloy with the thickness of 6mm to the thickness of 3mm at the temperature of 500 ℃, and then preserving heat for 36 hours at the temperature of 700 ℃; and finally, cleaning and drying the treated titanium-zirconium alloy by using an acetone solution. As shown in FIG. 5, the results of the test showed that a completely recrystallized structure with a clear boundary and a uniform crystal grain size was obtained.
The experimental methods described above are only embodiments of the present invention, and therefore, should not be construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (5)
1. A treatment process for obtaining a complete recrystallization structure of a low-zirconium-content titanium-zirconium alloy, wherein the mass percent of Zr in the low-zirconium-content titanium-zirconium alloy is less than or equal to 20 percent; the method comprises the following steps:
1) selecting titanium-zirconium alloy with low zirconium content as a heat treatment material;
2) carrying out acid pickling corrosion on the titanium-zirconium alloy by using a high-concentration corrosive liquid to remove surface oxide skin, and then cleaning and drying by using a cleaning liquid;
3) hot rolling the dried alloy below the alpha + beta/alpha transition temperature until the reduction rate is 50 percent;
4) carrying out first heat treatment on the titanium-zirconium alloy subjected to hot rolling treatment; the first heat treatment adopts vacuum furnace heat treatment, and the temperature is kept for 36 hours at 50 ℃ below the alpha + beta/alpha transition temperature;
5) carrying out warm rolling on the treated alloy below the alpha + beta/alpha transition temperature until the reduction rate is 50 percent;
6) carrying out secondary heat treatment on the titanium-zirconium alloy subjected to warm rolling treatment; the second heat treatment adopts vacuum furnace heat treatment, and the temperature is kept for 1 to 36 hours at 50 ℃ below the alpha + beta/alpha transition temperature;
7) and cleaning and drying the treated titanium-zirconium alloy by using a cleaning solution.
2. The process according to claim 1, characterized in that: the high-concentration corrosive liquid comprises HF and HNO in a volume ratio3:H2O=1：3：10。
3. The process according to claim 1, characterized in that: the cleaning solution in the step 2) and the cleaning solution in the step 7) are acetone solutions; and ultrasonic cleaning is adopted.
4. The process according to claim 1, characterized in that: the hot rolling process comprises the following steps: keeping the temperature below the alpha + beta/alpha transition temperature for 3min before rolling each time, slowly reducing the distance between two rollers of the rolling mill until the rolling reduction is 50 percent, and adopting unidirectional rolling.
5. The process according to claim 1, characterized in that: the warm rolling process comprises the following steps: keeping the temperature below 500 ℃ for 3min before each rolling, slowly reducing the distance between two rollers of a rolling machine until the rolling reduction rate is 50%, and adopting unidirectional rolling.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910290266.7A CN110042335B (en) | 2019-04-11 | 2019-04-11 | Treatment process for obtaining complete recrystallization structure of titanium-zirconium alloy with low zirconium content |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910290266.7A CN110042335B (en) | 2019-04-11 | 2019-04-11 | Treatment process for obtaining complete recrystallization structure of titanium-zirconium alloy with low zirconium content |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110042335A CN110042335A (en) | 2019-07-23 |
| CN110042335B true CN110042335B (en) | 2020-10-16 |
Family
ID=67276857
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910290266.7A Active CN110042335B (en) | 2019-04-11 | 2019-04-11 | Treatment process for obtaining complete recrystallization structure of titanium-zirconium alloy with low zirconium content |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110042335B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113521384B (en) * | 2021-07-05 | 2022-05-10 | 湖南湘投金天钛金属股份有限公司 | Titanium-based material and preparation method and application thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003003224A (en) * | 2001-06-20 | 2003-01-08 | Sumitomo Rubber Ind Ltd | High-strength titanium alloy material, method of manufacturing for the same and golf club head using the alloy material |
| CN105734474B (en) * | 2016-03-29 | 2017-05-24 | 浙江大学 | Treatment process used for improving cold rolling performance of titanium and zirconium alloy high in zirconium content |
| CN107916422B (en) * | 2017-10-31 | 2020-04-10 | 浙江大学 | Method for preparing porous bionic structure on surface of titanium-zirconium alloy |
-
2019
- 2019-04-11 CN CN201910290266.7A patent/CN110042335B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN110042335A (en) | 2019-07-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Kim et al. | Texture and shape memory behavior of Ti–22Nb–6Ta alloy | |
| Liu et al. | Mechanical properties and cytocompatibility of oxygen-modified β-type Ti–Cr alloys for spinal fixation devices | |
| WO2012032610A1 (en) | Titanium material | |
| CN112251639B (en) | High-strength antibacterial titanium alloy bar, high-strength antibacterial titanium alloy wire and preparation method of high-strength antibacterial titanium alloy bar | |
| EP3284836B1 (en) | Zirconium alloy having excellent corrosion resistance and creep resistance, and method for manufacturing same | |
| CN108977693B (en) | A kind of recrystallization high-strength titanium alloy and preparation method thereof | |
| CN105603258B (en) | A kind of high intensity zircaloy and preparation method | |
| CN114657417B (en) | High-strength plastic titanium alloy suitable for cold deformation processing and preparation method thereof | |
| US3492172A (en) | Method for producing titanium strip | |
| CN110042335B (en) | Treatment process for obtaining complete recrystallization structure of titanium-zirconium alloy with low zirconium content | |
| CN109797314B (en) | High-niobium TiAl alloy with nano-scale grains and preparation method thereof | |
| CN113817972B (en) | Method for arbitrarily adjusting equiaxial alpha phase content in titanium alloy through heat treatment | |
| CN111809081B (en) | High-strength and high-plasticity ZrTiAlNb zirconium titanium-based alloy and preparation method thereof | |
| CN108913943A (en) | Tough titanium alloy of a kind of nearly α phase height and preparation method thereof | |
| CN114635099A (en) | Continuous multi-step thermal hydrogen treatment process for optimizing TC21 titanium alloy microstructure | |
| JP5382518B2 (en) | Titanium material | |
| CN113549788A (en) | Double-state high-strength plastic-zirconium alloy and preparation method thereof | |
| JPS63230858A (en) | Manufacture of titanium-alloy sheet for superplastic working | |
| JPH04247856A (en) | Method for cold rolling of pure titanium | |
| CN115747690B (en) | Preparation method of close-packed hexagonal metal material containing ultra-high density twin crystals | |
| CN112553552B (en) | Processing technology for improving mechanical property of titanium-zirconium alloy, titanium-zirconium alloy and implant | |
| CN105734474B (en) | Treatment process used for improving cold rolling performance of titanium and zirconium alloy high in zirconium content | |
| CN113667914B (en) | Method for preparing high-strength pure zirconium through cold deformation | |
| RU2716928C1 (en) | Titanium-based alloy and its processing method for creating intraosseous implants with high biomechanical compatibility with bone tissue | |
| CN115261670B (en) | High-strength and high-toughness pure titanium and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |