CN112210680A - High-processability titanium alloy and preparation method thereof - Google Patents
High-processability titanium alloy and preparation method thereof Download PDFInfo
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- CN112210680A CN112210680A CN202011002304.3A CN202011002304A CN112210680A CN 112210680 A CN112210680 A CN 112210680A CN 202011002304 A CN202011002304 A CN 202011002304A CN 112210680 A CN112210680 A CN 112210680A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- 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
Abstract
A titanium alloy with high processability and a preparation method thereof belong to the technical field of metal smelting. In order to solve the problems of poor alloy processability, large deformation resistance and narrow processing window in the process of smelting titanium alloy by a liquid hydrogen-placing method, the invention provides a method for preparing a titanium alloy with high processability by dynamically hydrogen-placing alloy titanium melt, which comprises the following steps: weighing raw materials according to the proportion of each component of the titanium alloy, and placing the raw materials in a crucible; adjusting the vacuum degree of the smelting chamber to be less than 5 multiplied by 10‑3Pa; filling mixed gas of hydrogen and argon into the smelting chamber until the gas pressure in the smelting chamber is 10KPa-50KPa, keeping the pressure constant, wherein the flow ratio of the hydrogen to the argon is 1: (1-20), smelting for 1min-30min under the condition that the smelting current is 150A-800A, and repeatedly smelting for 3-8 times to finish smelting to obtain the titanium alloy. The invention has high efficiency, low energy consumption and strong economic and practical value.
Description
Technical Field
The invention relates to the technical field of metal smelting, and provides a titanium alloy with high processability and a preparation method thereof.
Background
With the continuous development of the aerospace field, the demand for various aerospace structural members with excellent performance is increasing, wherein titanium alloy is widely applied with excellent performance, but the titanium alloy has low room temperature plasticity, low deformation limit, large deformation resistance, easy cracking during cold forming and narrow hot processing window, and the processing and application of the titanium alloy are greatly limited. The hot hydrogen treatment technology is started in the middle of the last century, and the main idea is to improve the microstructure of refined titanium alloy by taking hydrogen as a temporary alloy element, induce dislocation motion and dynamic recrystallization of the titanium alloy, improve the processing performance of the titanium alloy in the hot processing procedure of titanium alloy castings and cast ingots, and further prepare aerospace structural parts with various complex shapes. The titanium alloy is subjected to dehydrogenation through vacuum heat treatment before use so as to avoid hydrogen embrittlement.
The traditional thermal hydrogen treatment method is that the titanium alloy is heated to a certain temperature after being introduced with hydrogen atmosphere in a heat treatment furnace and is kept warm for a period of time, hydrogen molecules are dissociated into hydrogen atoms on the surface of the alloy, and hydrogen elements are diffused into the alloy by utilizing the hydrogen concentration gradient in the titanium alloy. Since the hydrogen is always introduced while the titanium alloy is in the solid state in this process, this method is called solid-state hydrogen introduction. The solid hydrogen placement has the defects of low diffusion speed, low hydrogen placement efficiency and high energy consumption, can only process thin-wall parts, has high hydrogen placement amount but can react with titanium to generate brittle hydride phases, and has adverse effect on the deformation of the titanium alloy. In recent years, a liquid hydrogen method has been developed in which a titanium alloy is melted in a mixed atmosphere by introducing a fixed amount of hydrogen-argon mixed gas into a vacuum melting furnace. Since the titanium alloy is always in a molten state, it is called liquid hydrogen storage. However, the titanium alloy prepared by the existing liquid hydrogen-placing method has poor hot-working performance.
Disclosure of Invention
In order to solve the problems of poor alloy processability, large deformation resistance and narrow processing window in the process of smelting titanium alloy by a liquid hydrogen-placing method, the invention provides a method for preparing a titanium alloy with high processability by dynamically hydrogen-placing alloy titanium melt, which comprises the following steps:
1) raw material feeding: weighing raw materials according to the proportion of each component of the titanium alloy, and placing the raw materials in a crucible;
2) vacuumizing: adjusting the vacuum degree of the smelting chamber to be less than 5 multiplied by 10-3Pa；
3) Introducing a dynamic atmosphere: filling mixed gas of hydrogen and argon into the smelting chamber until the gas pressure in the smelting chamber is 10KPa-50KPa, keeping the pressure constant, wherein the flow ratio of the hydrogen to the argon is 1: (1-20);
4) smelting: smelting for 1min-30min under the condition that the smelting current is 150A-800A, and repeatedly smelting for 3-8 times to finish smelting to obtain the titanium alloy.
Further limiting, before weighing each raw material of the titanium alloy in the step 1), removing oil stains on the surface by using an organic solvent, and then drying for 1h in a drying oven at 200 ℃.
More specifically, the organic solvent is absolute ethyl alcohol, acetone or petroleum ether.
Further, the titanium alloy in step 1) is industrially pure titanium, a near-alpha type titanium alloy, an alpha + beta type titanium alloy, a metastable beta type titanium alloy or a beta type titanium alloy.
Further, the vacuum degree in the step 2) is 4.0 x 10-3Pa。
Further, in the step 3), the flow ratio of the hydrogen to the argon is 1: 4.
further limiting, the mixed gas is continuously introduced into the smelting chamber in the smelting process in the step 3).
Further defining, step 4) said melting: smelting under the condition of 200A for 5min, and repeatedly smelting for 4 times.
The invention also provides the high-processability titanium alloy obtained by the preparation method, wherein the hydrogen content of the high-processability titanium alloy is 200-1400 wppm (mass million fraction, namely 2.00 multiplied by 10)-2wt.％-14.00×10-2wt.％)。
Advantageous effects
The titanium alloy obtained by the invention has high hydrogen content, and is very suitable for further hot working and forming of cast ingots at lower temperature and lower pressure so as to reduce the energy consumption of hot working.
The invention provides a novel, simple and practical preparation method for preparing the titanium alloy with high processability, and the hot processing performance of the titanium alloy can be greatly improved by regulating and controlling the hydrogen storage amount of the titanium alloy. The invention has high efficiency, low energy consumption and strong economic and practical value.
Detailed Description
The technical solution of the present invention is not limited to the following specific embodiments, but includes any combination of the specific embodiments.
According to the invention, the alloy is smelted by using the vacuum non-consumable arc furnace under the hydrogen-argon mixed atmosphere, so that the hydrogen-argon mixed gas in the vacuum chamber is dynamically input all the time, the hydrogen and argon (1: 1-1: 20) can be mixed in any proportion, the high hydrogen content in the alloy can be further achieved, and the titanium alloy with high processing performance can be obtained. The scheme of the present invention is described in detail below:
example 1. method of making high processability titanium alloy.
1) Raw material feeding: cleaning sponge titanium which is a raw material of industrial pure titanium Ti in absolute ethyl alcohol which is an organic solvent to remove surface oil stains, drying the sponge titanium in a drying oven for 1 hour at 200 ℃ to remove water in the raw material, and then placing the raw material in a water-cooled copper crucible.
2) Vacuumizing: closing the furnace door, and sequentially starting the mechanical pump and the molecular pump to make the vacuum degree of the vacuum melting chamber reach 4.0 multiplied by 10-3Pa。
3) Introducing a dynamic atmosphere: opening atmosphere control system, opening the gas valve, fill hydrogen and argon gas into the gas-mixing chamber through the intake manifold way, adjust hydrogen and argon gas flow ratio through the relief pressure valve and be 1: 4. the flow rate of the gas entering the gas mixing chamber is controlled by a valve, so that the hydrogen and the argon are filled into the gas mixing chamber at a constant flow rate, and the flow rate of the hydrogen and the argon is checked at any time by adopting a digital pressure flow meter in the gas mixing chamber. And the mixed gas in the gas mixing chamber enters the vacuum melting chamber through a pumping system. The top of the electric arc furnace is provided with a digital pressure sensor for detecting the gas pressure of the vacuum melting chamber to ensure that the gas pressure of the melting chamber is always 50KPa, once the pressure exceeds the value, the one-way pressure relief valve is opened, and redundant gas is discharged through a gas outlet pipeline. In the processes of alloy smelting and alloy solidification cooling, the atmosphere control system is kept open all the time, and the mixed gas is continuously introduced into the smelting chamber, so that the flow ratio of hydrogen and argon in the mixed gas can be adjusted at any time, and the purpose of regulating and controlling the hydrogen content in the titanium melt is achieved.
4) Smelting: and (4) turning on a power supply, and starting to smelt by striking an arc through an electrode. Smelting current is 200A, smelting for 5min each time, remelting for 4 times, turning off a power supply, and stopping smelting. And taking out the alloy ingot after solidification and cooling, and closing the atmosphere control system.
Example 2. example 1 was repeated, except that the alloy described in this example was an α + β type titanium alloy and the composition was Ti-6 Al-4V.
Example 3. example 1 was repeated, which is different from example 1 in that the gas pressure in the melting furnace in step 3) in this example was 10Kpa, and the flow ratio of hydrogen to argon was 1: 5.
example 4. example 1 was repeated, which is different from example 1 in that the gas pressure in the melting furnace in step 3) in this example was 25Kpa, and the flow ratio of hydrogen to argon was 1: 1.
example 5. example 1 was repeated, which is different from example 1 in that the melting current in step 4) was 150A, and the melting time was 30 min.
Example 6. example 1 was repeated, which is different from example 1 in that the melting current in step 4) was 500A for 15min each time.
Example 7. example 1 was repeated, which is different from example 1 in that the melting current in step 4) was 800A for 1min per melting.
Example 8 example 1 was repeated, which is different from example 1 in that the pressure of the gas in the melting furnace in step 3) was 50Kpa, the flow ratio of hydrogen to argon was 1: 1.
example 9. example 1 was repeated, which is different from example 1 in that the pressure of the gas in the melting furnace in step 3) was 50Kpa, the flow ratio of hydrogen to argon was 1: 20.
the following is a study of the processing properties of the titanium alloy obtained by the preparation method of the present invention.
Example 10. high processability titanium alloy, labeled a, prepared as follows:
1) raw material feeding: sponge titanium, pure aluminum particles and aluminum-vanadium intermediate alloy particles which are raw materials of alpha + beta type titanium alloy Ti-6Al-4V are cleaned in absolute ethyl alcohol which is an organic solvent to remove surface oil stains, and are dried in a drying oven at 200 ℃ for 1h to remove water in the raw materials, then the raw materials are weighed according to the alloy component proportion, and the raw materials are placed in a water-cooled copper crucible.
2) Vacuumizing: closing the furnace door, and sequentially starting the mechanical pump and the molecular pump to make the vacuum degree of the vacuum melting chamber reach 5 x 10- 3Pa。
3) Introducing a dynamic atmosphere: opening atmosphere control system, opening the gas valve, fill hydrogen and argon gas into the gas-mixing chamber through the intake manifold way, adjust hydrogen and argon gas flow ratio through the relief pressure valve and be 1: 9. the flow rate of the gas entering the gas mixing chamber is controlled by a valve, so that the hydrogen and the argon are filled into the gas mixing chamber at a constant flow rate of 25L/min, and the flow rate of the hydrogen and the argon is checked at any time by adopting a digital pressure flow meter in the gas mixing chamber. And the mixed gas in the gas mixing chamber enters the vacuum melting chamber through a pumping system. The top of the electric arc furnace is provided with a digital pressure sensor for detecting the gas pressure of the vacuum melting chamber to ensure that the gas pressure of the melting chamber is always 50KPa, once the pressure exceeds the value, the one-way pressure relief valve is opened, and redundant gas is discharged through a gas outlet pipeline. In the invention, the atmosphere control system is always kept on in the alloy smelting and alloy solidification cooling processes.
4) Smelting: and (4) turning on a power supply, and starting to smelt by striking an arc through an electrode. Smelting current is 200A, smelting for 5min each time, remelting for 4 times, turning off a power supply, and stopping smelting. And taking out the alloy ingot after solidification and cooling, and closing the atmosphere control system.
Comparative example: the titanium alloy with the same mass and the same components as those of the alloy A is marked as B, and the preparation method comprises the following steps:
1) raw material feeding: sponge titanium, pure aluminum particles and aluminum vanadium alloy particles which are used as raw materials of alpha + beta type titanium alloy Ti-6Al-4V are cleaned in absolute ethyl alcohol which is an organic solvent to remove surface oil stains, and are dried in a drying oven at 200 ℃ for 1 hour to remove water in the raw materials, then the raw materials are weighed according to the alloy component proportion, and the raw materials are placed in a water-cooled copper crucible.
2) Vacuumizing: closing the furnace door, and sequentially starting the mechanical pump and the molecular pump to make the vacuum degree of the vacuum melting chamber reach 5 x 10- 3Pa。
3) And opening an atmosphere control system, opening a gas valve, filling pure argon into the gas mixing chamber through the gas inlet pipeline, controlling the flow rate of the gas entering the gas mixing chamber through the valve, filling the argon into the gas mixing chamber at a constant flow rate of 25L/min, and checking the gas flow rate of the argon at any time by adopting a digital pressure flow meter in the gas mixing chamber. And the gas in the gas mixing chamber enters the vacuum smelting chamber through a pumping system. The top of the electric arc furnace is provided with a digital pressure sensor for detecting the gas pressure of the vacuum melting chamber to ensure that the gas pressure of the melting chamber is always 50KPa, once the pressure exceeds the value, the one-way pressure relief valve is opened, and redundant gas is discharged through a gas outlet pipeline. In the invention, the atmosphere control system is always kept on in the alloy smelting and alloy solidification cooling processes.
4) Smelting: and (4) turning on a power supply, and starting to smelt by striking an arc through an electrode. Smelting current is 200A, smelting for 5min each time, remelting for 4 times, turning off a power supply, and stopping smelting. And taking out the alloy ingot after solidification and cooling, and closing the atmosphere control system.
The hot working process of two titanium alloys was simulated using a dynamic thermal simulation tester, and the hot-compressed samples were taken from example 10 (denoted as alloy a) and comparative example (denoted as alloy B), respectively, and had a phi 6 x 9mm cylinder size. The thermal compression experiment is carried out on a Gleeble-1500D dynamic thermal simulation testing machine, the heating rate is 10K/s, the temperature is kept for 3 minutes, the lubricity of the sample in contact with a pressure head is guaranteed by graphite gaskets at two ends of the sample, the sample is protected by high-temperature silica gel, the deformation temperature is measured by a thermocouple, the deformation is 50%, and the protective gas is argon.
Using strain rate 0.01s-1The thermal compression temperature was set to 700, 750, 800 and 850 deg.C, and the thermal compression temperature was set to 850 deg.CStrain rates of 0.1s, respectively-1、0.01s-1And 0.001s-1The experimental conditions of (1). The results are shown in the table.
TABLE 1 thermal compression temperatures 700, 750, 800, 850 ℃ and strain rates 0.01s-1Peak flow stress of alloys A and B
TABLE 2 thermal compression temperature 850 ℃ and strain rate 0.1s-1、0.01s-1、0.001s-1Peak flow stress of alloys A and B
The strain rate was 0.01s at 700, 750, 800 and 850 ℃ thermal compression temperature, respectively-1The peak rheological stresses for the a and B alloys under the experimental conditions of (a) and (B) are shown in table 1. The alloy A obtained by the preparation method of the invention has the strain rate of 0.01s-1Under the same temperature, the peak value rheological stress during hot processing is lower than that of the B alloy which is not prepared by the method, and the high processing performance of the titanium alloy obtained by the preparation method is shown.
The strain rates were 0.1s at a thermocompression temperature of 850 deg.C-1、0.01s-1And 0.001s-1The peak flow stress of the resulting alloy a and B is shown in table 2. The alloy A obtained by the preparation method has lower peak value rheological stress in hot processing than the alloy B which is not prepared by the method under the same strain rate that the hot compression temperature is 850 ℃, and shows the high processing performance of the titanium alloy obtained by the preparation method.
Properties of titanium alloys prepared by the methods of examples 1 to 10, hot compression temperature 850 deg.C for 0.1s-1The strain rate is used for detecting the peak value rheological stress of the titanium alloy prepared by the method, and the hydrogen content of the prepared titanium alloy is detected by a combustion method. Statistics knotAs shown in table 3.
TABLE 3 statistics of hydrogen content and processability of titanium alloys prepared by the method of the invention
Claims (9)
1. The preparation method of the titanium alloy with high processability is characterized by comprising the following steps:
1) raw material feeding: weighing raw materials according to the proportion of each component of the titanium alloy, and placing the raw materials in a crucible;
2) vacuumizing: adjusting the vacuum degree of the smelting chamber to be less than 5 multiplied by 10-3Pa；
3) Introducing a dynamic atmosphere: filling mixed gas of hydrogen and argon into the smelting chamber until the gas pressure in the smelting chamber is 10KPa-50KPa, keeping the pressure constant, wherein the flow ratio of the hydrogen to the argon is 1: (1-20);
4) smelting: smelting for 1min-30min under the condition that the smelting current is 150A-800A, and repeatedly smelting for 3-8 times to finish smelting to obtain the titanium alloy.
2. The preparation method of claim 1, wherein the titanium alloy raw materials in the step 1) are degreased on the surface by using an organic solvent before being weighed, and then are dried in a drying oven at 200 ℃ for 1 h.
3. The method according to claim 2, wherein the organic solvent is absolute ethanol, acetone, or petroleum ether.
4. The method according to claim 1, wherein the titanium alloy of step 1) is commercially pure titanium, a near- α type titanium alloy, an α + β type titanium alloy, a metastable β type titanium alloy, or a β type titanium alloy.
5. The method according to claim 1, wherein the degree of vacuum in step 2) is 4.0X 10-3Pa。
6. The method according to claim 1, wherein the flow ratio of hydrogen to argon in step 3) is 1: 4.
7. the preparation method of claim 1, wherein the mixed gas is continuously introduced into the smelting chamber during the smelting in the step 3).
8. The method of claim 1, wherein step 4) said melting: smelting under the condition of 200A for 5min, and repeatedly smelting for 4 times.
9. The high-processability titanium alloy obtained by the preparation method of any one of claims 1 to 8, wherein the hydrogen content of the high-processability titanium alloy is 200 to 1400 wppm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112899517A (en) * | 2021-01-18 | 2021-06-04 | 哈尔滨工业大学 | Method for improving thermal deformation performance of titanium-based composite material |
| CN114635099A (en) * | 2022-03-23 | 2022-06-17 | 合肥工业大学 | Continuous multi-step thermal hydrogen treatment process for optimizing TC21 titanium alloy microstructure |
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