CN110306139B - Continuous multi-step thermal hydrogen treatment process for improving room temperature plasticity of TC4 titanium alloy - Google Patents
Continuous multi-step thermal hydrogen treatment process for improving room temperature plasticity of TC4 titanium alloy Download PDFInfo
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- CN110306139B CN110306139B CN201910742808.XA CN201910742808A CN110306139B CN 110306139 B CN110306139 B CN 110306139B CN 201910742808 A CN201910742808 A CN 201910742808A CN 110306139 B CN110306139 B CN 110306139B
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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
Abstract
The invention discloses a continuous multi-step thermal hydrogen treatment process for improving the room temperature plasticity of TC4 titanium alloy, which comprises the steps of firstly carrying out surface treatment on a TC4 titanium alloy sample, then heating the sample to a hydrogen charging temperature in a vacuum environment, then continuously charging hydrogen in multiple steps, at least preserving the temperature until the hydrogen pressure is stable after each step of charging hydrogen, and finally air-cooling to the room temperature after the last step of charging hydrogen, thus finishing the improvement of the room temperature plasticity of the TC4 titanium alloy. The method is simple and easy to implement, low in cost and obvious in plasticizing effect, and the room temperature plasticity of the treated TC4 titanium alloy is obviously improved, so that the room temperature plastic forming of the TC4 titanium alloy complex structural member is facilitated, and the application range of the TC4 titanium alloy can be expanded.
Description
Technical Field
The invention belongs to the field of titanium alloy material treatment, and particularly relates to a titanium alloy heat treatment process.
Background
At present, titanium alloy is widely applied to the fields of aviation, aerospace and the like due to a series of excellent properties such as high specific strength, good high temperature resistance, good corrosion resistance, no magnetism and the like. The TC4 titanium alloy is an alpha + beta type titanium alloy, has good comprehensive performance, and is the most widely applied titanium alloy at home and abroad at present. However, the TC4 titanium alloy has low plasticity at room temperature, low deformation limit, and is easily cracked during cold forming, which limits its room temperature plastic forming. Most titanium alloys currently require plastic forming at high temperatures. Although titanium alloys have good plastic formability at high temperatures, high temperatures also present a series of problems to forming: high deformation temperature, large flow stress, difficult control of microstructure and performance and high requirements on dies and forming equipment. In addition, the protection of raw materials, systems and processes from high temperatures is difficult.
In recent years, the thermal hydrogen treatment technology is widely applied to improve the structure and the performance of the titanium alloy. The hot hydrogen treatment technology is to improve the room temperature structure, mechanical property, processing property and the like of the titanium alloy by taking hydrogen as a temporary alloy element and utilizing hydrogen induced plasticity, hydrogen induced phase change and reversible alloying action of the hydrogen in the titanium alloy. Finally, according to the reversible alloying action of hydrogen in the titanium alloy, the hydrogen in the alloy is removed by using a vacuum annealing method so as to prevent the hydrogen embrittlement of the alloy in the using process.
At present, a hydrogen treatment process for improving the room temperature plasticity of the titanium alloy is relatively complex, and the existing hot hydrogen treatment process for improving the room temperature plasticity of the titanium alloy generally comprises the steps of firstly carrying out hydrogen treatment on a titanium alloy sample, and then carrying out solution quenching treatment on the hydrogen-titanium alloy sample, so that a beta phase with good plasticity is kept to the room temperature, and the room temperature plasticity of the titanium alloy is improved. However, titanium alloys are easily oxidized at high temperatures, and hydrogen escapes from hydrogenated titanium alloys at high temperatures. Therefore, when the hydrogen titanium alloy sample is subjected to solution quenching treatment, the hydrogen titanium alloy sample needs to be vacuum-sealed in a quartz tube, so that oxidation of the hydrogen titanium alloy sample and escape of a large amount of hydrogen can be avoided. However, for the hydrogen-containing titanium alloy sample with larger volume and mass, the vacuum packaging and the solution quenching treatment of the sample are more difficult.
Disclosure of Invention
Aiming at the complexity of the existing hot hydrogen treatment process for improving the room temperature plasticity of the titanium alloy, the invention aims to provide a continuous multi-step hot hydrogen treatment process for improving the room temperature plasticity of the TC4 titanium alloy, so that the room temperature plasticity of the TC4 titanium alloy can be effectively improved in a simpler and more convenient mode.
In order to realize the purpose of the invention, the following technical scheme is adopted:
a continuous multi-step thermal hydrogen treatment process for improving room temperature plasticity of TC4 titanium alloy is characterized in that: firstly, carrying out surface treatment on a TC4 titanium alloy sample, then heating the sample to a hydrogen charging temperature in a vacuum environment, continuously charging hydrogen in multiple steps, carrying out heat preservation at least until the hydrogen pressure is stable after each step of charging hydrogen, and carrying out air cooling to room temperature after the last step of charging hydrogen, thus finishing the improvement of room temperature plasticity of the TC4 titanium alloy. The method specifically comprises the following steps:
step 1, polishing a TC4 titanium alloy sample by using abrasive paper, performing ultrasonic cleaning in absolute ethyl alcohol, and then drying to ensure that the surface of the sample is free of pollution;
step 2, placing the sample into a furnace tube of a tube furnace, starting a vacuum system, and vacuumizing the furnace tube; starting to heat, and closing a vacuum valve of the vacuum system when the temperature rises to the hydrogen charging temperature;
step 3, filling hydrogen into the furnace tube, and at least preserving heat until the hydrogen pressure in the furnace tube is stable, wherein the number of steps of filling hydrogen at the moment is recorded as 1 step;
step 4, after the heat preservation of the previous step is finished, filling hydrogen into the furnace tube again, and preserving heat at least until the hydrogen pressure in the furnace tube is stable, wherein the number of hydrogen filling steps is + 1;
step 5, repeating the step 4 until the required hydrogen filling steps are reached;
and 6, after the hydrogen filling is finished, cooling the sample in air to room temperature, and taking out the sample to finish the improvement of the room temperature plasticity of the TC4 titanium alloy.
Further, in step 2, the vacuum pumping is performed until the vacuum degree in the furnace tube is lower than 1.5 × 10-3Pa。
Further, in step 2, the charging temperature is 750-.
Further, in the step 3, hydrogen is filled until the hydrogen pressure in the furnace tube is-0.08 MPa, and the heat preservation time is 1 h.
Further, in the step 4, 0.008MPa of hydrogen is filled in each step, and the heat preservation time is 1 h.
Further, in step 5, the required number of hydrogen charging steps is 4-12.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention provides a continuous multi-step thermal hydrogen treatment process, which increases the volume fraction of a TC4 titanium alloy plastic phase, enables more beta phases to be reserved to room temperature, obviously improves the room temperature plasticity of the TC4 titanium alloy, is beneficial to room temperature plastic forming of a TC4 titanium alloy complex structural part, and can expand the application range of the TC4 titanium alloy.
2. The method does not need solution quenching treatment, avoids vacuum packaging of the hydrogen-containing titanium alloy sample in a quartz tube, can reduce the difficulty of the titanium alloy hot hydrogen treatment process, and is particularly obvious for titanium alloy samples with larger volume and mass; the invention reduces the investment of vacuum packaging processing links and packaging equipment, improves the efficiency, reduces the cost, is simple and easy to implement, and has good application and popularization values.
Detailed Description
The embodiments related to the present invention are specifically illustrated below by examples, which are only limited examples for illustrating the embodiments of the present invention and do not limit the scope of the present invention.
Example 1
Step 1, polishing a TC4 titanium alloy sample by using abrasive paper, performing ultrasonic cleaning in absolute ethyl alcohol, and then drying to ensure that the surface of the sample is free of pollution;
step 2, placing the sample into a furnace tube of the tube furnace, starting a vacuum system, and vacuumizing until the vacuum degree in the furnace tube is lower than 1.5 multiplied by 10-3Pa; starting to heat up at the speed of 10 ℃/min, and closing a vacuum valve at the end of the vacuum system when the temperature rises to 750 ℃;
step 3, filling hydrogen into the furnace tube to-0.08 MPa, preserving the heat for 1 hour, and recording the number of hydrogen filling steps as 1 step;
step 4, after the heat preservation of the previous step is finished, filling hydrogen into the furnace tube again, wherein the hydrogen of 0.008MPa is filled in the step, and the heat preservation is carried out for 1 hour, wherein the number of the hydrogen filling steps is plus 1;
step 5, repeating the step 4 until the number of the hydrogen filling steps is 8;
and 6, after the hydrogen charging is finished, cooling the sample to room temperature in air, taking out the sample, and obtaining the detection result of the plasticity index shown in the table 1.
Example 2
Step 1, polishing a TC4 titanium alloy sample by using abrasive paper, performing ultrasonic cleaning in absolute ethyl alcohol, and then drying to ensure that the surface of the sample is free of pollution;
step 2, placing the sample into a furnace tube of the tube furnace, starting a vacuum system, and vacuumizing until the vacuum degree in the furnace tube is lower than 1.5 multiplied by 10-3Pa; starting to heat up at the speed of 10 ℃/min, and closing a vacuum valve at the end of the vacuum system when the temperature rises to 800 ℃;
step 3, filling hydrogen into the furnace tube to-0.08 MPa, preserving the heat for 1 hour, and recording the number of hydrogen filling steps as 1 step;
step 4, after the heat preservation of the previous step is finished, filling hydrogen into the furnace tube again, wherein the hydrogen of 0.008MPa is filled in the step, and the heat preservation is carried out for 1 hour, wherein the number of the hydrogen filling steps is plus 1;
step 5, repeating the step 4 until the number of the hydrogen filling steps is 4;
and 6, after the hydrogen charging is finished, cooling the sample to room temperature in air, taking out the sample, and obtaining the detection result of the plasticity index shown in the table 1.
Example 3
Step 1, polishing a TC4 titanium alloy sample by using abrasive paper, performing ultrasonic cleaning in absolute ethyl alcohol, and then drying to ensure that the surface of the sample is free of pollution;
step 2, placing the sample into a furnace tube of the tube furnace, starting a vacuum system, and vacuumizing until the vacuum degree in the furnace tube is lower than 1.5 multiplied by 10-3Pa; starting to heat up at the speed of 10 ℃/min, and closing a vacuum valve at the end of a vacuum system when the temperature rises to 850 ℃;
step 3, filling hydrogen into the furnace tube to-0.08 MPa, preserving the heat for 1 hour, and recording the number of hydrogen filling steps as 1 step;
step 4, after the heat preservation of the previous step is finished, filling hydrogen into the furnace tube again, wherein the hydrogen of 0.008MPa is filled in the step, and the heat preservation is carried out for 1 hour, wherein the number of the hydrogen filling steps is plus 1;
step 5, repeating the step 4 until the number of the hydrogen filling steps is 11;
and 6, after the hydrogen charging is finished, cooling the sample to room temperature in air, taking out the sample, and obtaining the detection result of the plasticity index shown in the table 1.
TABLE 1 results of testing room temperature plasticity index of original TC4 titanium alloy treated by different continuous multi-step thermal hydrogen treatment processes
| Test specimen | Ultimate rate of deformation/%) | Increased amplitude/% over the original sample |
| Original | 17.16 | / |
| Example 1 | 23.88 | 39.16 |
| Example 2 | 27.59 | 60.78 |
| Example 3 | 34.07 | 98.54 |
Note: the room temperature compression experiment was carried out on MTS Landmark type equipment at a compression rate of 0.5 mm/min.
The above description is only exemplary of the present invention and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (3)
1. A continuous multi-step thermal hydrogen treatment process for improving room temperature plasticity of TC4 titanium alloy is characterized in that: firstly, performing surface treatment on a TC4 titanium alloy sample, then heating the sample to a hydrogen charging temperature in a vacuum environment, continuously charging hydrogen in multiple steps, preserving the temperature at least until the hydrogen pressure is stable after each step of hydrogen charging, and performing air cooling to room temperature after the last step of hydrogen charging, namely completing the improvement of room temperature plasticity of the TC4 titanium alloy; the method specifically comprises the following steps:
step 1, polishing a TC4 titanium alloy sample by using abrasive paper, performing ultrasonic cleaning in absolute ethyl alcohol, and then drying to ensure that the surface of the sample is free of pollution;
step 2, placing the sample into a furnace tube of a tube furnace, starting a vacuum system, and vacuumizing the furnace tube; starting temperature rise at the temperature rise rate of 10 ℃/min, and closing a vacuum valve of the vacuum system when the temperature rises to the hydrogen charging temperature of 750-;
step 3, filling hydrogen into the furnace tube until the hydrogen pressure in the furnace tube is-0.08 MPa, and preserving heat for 1h to stabilize the hydrogen pressure in the furnace tube, wherein the number of hydrogen filling steps is marked as 1 step;
step 4, after the heat preservation of the previous step is finished, filling 0.008MPa hydrogen into the furnace tube again, preserving the heat for 1 hour to ensure that the hydrogen pressure in the furnace tube is stable, wherein the number of the hydrogen filling steps is plus 1;
step 5, repeating the step 4 until the required hydrogen filling steps are reached;
and 6, after the hydrogen filling is finished, cooling the sample in air to room temperature, and taking out the sample to finish the improvement of the room temperature plasticity of the TC4 titanium alloy.
2. The continuous multi-step thermal hydrogen treatment process according to claim 1, characterized in that: in step 2, the vacuum pumping is performed until the vacuum degree in the furnace tube is lower than 1.5 multiplied by 10-3Pa。
3. The continuous multi-step thermal hydrogen treatment process according to claim 1, characterized in that: in step 5, the required hydrogen filling steps are 4-12 steps.
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