CN110972521B - Preparation method of near α type low-temperature titanium alloy pipe - Google Patents
Preparation method of near α type low-temperature titanium alloy pipe Download PDFInfo
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- CN110972521B CN110972521B CN201110011936.0A CN201110011936A CN110972521B CN 110972521 B CN110972521 B CN 110972521B CN 201110011936 A CN201110011936 A CN 201110011936A CN 110972521 B CN110972521 B CN 110972521B
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Abstract
The invention relates to a preparation method of a near α type low-temperature titanium alloy pipe, which is characterized in that the preparation process comprises the steps of (1) carrying out large-deformation cogging rolling on a low-temperature titanium alloy pipe blank, (2) carrying out vacuum heat treatment to obtain a cold-rolled pipe blank, (3) carrying out cold rolling on the cold-rolled pipe blank to obtain a finished pipe blank, (4) carrying out vacuum heat treatment at the temperature of 5-25 ℃ below the transition temperature of α - β, (5) carrying out 1-pass cold rolling on the finished pipe blank after heat treatment, and carrying out oil removal, acid cleaning and vacuum heat treatment to obtain the finished pipe.
Description
Technical Field
A preparation method of a near α type low-temperature titanium alloy pipe relates to a manufacturing method of a titanium alloy pipe used in the fields of aerospace, aviation, energy, chemical engineering and the like under the working conditions of low temperature and high pressure.
Background
With the vigorous development of aerospace industry in China, higher requirements are put forward on the use amount and comprehensive performance of titanium alloy pipes which are used under low temperature conditions and have light weight, high strength, low thermal conductivity and small expansion coefficient, the titanium alloy pipes are required to have excellent low-temperature strong plasticity matching, and the titanium alloy pipes are required to have excellent mechanical property and process property at room temperature, so that the titanium alloy pipes are suitable for being cold-formed into space structural members for pipeline systems with various complex shapes.
At present, titanium alloys commonly used in low-temperature application comprise pure titanium, full α titanium alloy TA1-TA7, near α titanium alloy TA7-TA24, α + β type titanium alloy TC4 and the like, wherein the full α and near α titanium alloys have good plasticity even at the temperature of liquid nitrogen (77K) and liquid hydrogen (20K) and have good weldability, and compared with α + β and β type titanium alloys, the titanium alloys have wider application at a low temperature, the near α type titanium alloys generally adopt a special high-temperature heat treatment mode to obtain good low-temperature performance, but simultaneously sacrifice the excellent room-temperature plasticity of the titanium alloys, so that the cold forming performance of the pipes at room temperature is poor, and simultaneously, the phenomena of drawing marks, folding and cracking of the surfaces of bent pipes are easily generated in the subsequent multidirectional space forming process, so that the sample processing is difficult.
Although the pipe produced by the preparation method of the low-temperature titanium alloy related to the nearly α type low-temperature titanium alloy and the preparation method thereof in the Chinese national defense patent ZL 03105962.7 has excellent low-temperature mechanical properties, the finished pipe has high vacuum heat treatment temperature and complex heat treatment system, and is easy to cause large pipe dimensional tolerance, large crystal grains and reduced room-temperature mechanical properties, so that the finished product rate is reduced, and the low-temperature titanium alloy is not suitable for engineering batch production.
Disclosure of Invention
The invention aims to provide a preparation method of a near α type low-temperature titanium alloy pipe, which can effectively improve the low-temperature comprehensive performance of a low-temperature titanium alloy pipe chamber, greatly improve the dimensional accuracy and the yield of finished pipes and meet the requirements of engineering mass production, aiming at the defects of the prior art.
In order to achieve the above object, the present invention adopts the following technical solutions.
A preparation method of a near α type low-temperature titanium alloy pipe is characterized by comprising the following steps:
(1) after surface scraping and boring treatment, the low-temperature titanium alloy tube blank is sent into a cogging mill for 1-2 times of large-deformation cogging rolling, and the pass deformation is controlled to be 35-60%;
(2) carrying out vacuum heat treatment on the cogging pipe at 650-750 ℃ for 1-2.5 hours, boring, scraping and removing oxide layers on the inner and outer surfaces to obtain a cold-rolled pipe blank;
(3) cold rolling the cold-rolled tube blank on a five-roller or three-roller finishing mill for 1-3 passes, and performing vacuum heat treatment at 650-750 ℃ in each pass to obtain a finished tube blank;
(4) carrying out vacuum heat treatment on the finished pipe blank at the temperature of 5-25 ℃ below the conversion temperature of α - β and the heat preservation time of 0.5-1 hour;
(5) and (3) carrying out 1-pass cold rolling on the finished pipe blank after heat treatment, controlling the pass deformation to be 25-45%, and carrying out oil removal, acid pickling and vacuum heat treatment at 650-750 ℃ to obtain the finished pipe.
The invention discloses a preparation method of a near α type low-temperature titanium alloy pipe, which is characterized in that a low-temperature titanium alloy pipe blank adopts a cross-rolled perforated pipe as a pipe blank, or adopts a pipe which is sheathed and extruded by a pipe and is machined by a forging machine as a pipe blank.
The invention discloses a preparation method of a near α type low-temperature titanium alloy pipe, which is characterized in that the boring is to remove the inner wall defects including cracks and pits, and the deviation of the wall thickness of a pipe blank is less than 0.50 mm.
The preparation method of the near α type low-temperature titanium alloy pipe is characterized in that the α - β transformation temperature of the low-temperature titanium alloy is 900-1200 ℃.
The invention discloses a preparation method of a near α type low-temperature titanium alloy pipe, which is characterized in that the vacuum degree of a finished pipe blank is not lower than 1 multiplied by 10 when the finished pipe blank is subjected to vacuum heat treatment-1Pa, and the temperature deviation of the hearth is within +/-5 ℃.
The invention discloses a preparation method of a near α type low-temperature titanium alloy pipe, which is characterized in that the cooling speed of a finished pipe blank is lower than 40 ℃/h when the finished pipe blank is subjected to vacuum heat treatment.
The invention discloses a preparation method of a near α type low-temperature titanium alloy pipe, which is characterized in that pickling solution for pickling comprises 21-30% of nitric acid and 7-10% of hydrofluoric acid by volume ratio, and the balance of water.
The invention discloses a preparation method of a near α type low-temperature titanium alloy pipe, which is characterized in that the specification of a finished pipe is phi 15-120 multiplied by 1-10 mm.
The invention discloses a preparation method of a near α type low-temperature titanium alloy pipe, which is characterized in that the microstructure of a finished pipe is an equiaxial α structure or an equiaxial α + small amount of sheet-shaped α structures.
The preparation method of the near α type low-temperature titanium alloy pipe is characterized in that the room-temperature tensile strength of a finished pipe is not less than 600MPa, the yield strength is not less than 480MPa, and the elongation after fracture is not less than 14%.
The invention discloses a preparation method of a near α type low-temperature titanium alloy pipe, which is characterized in that the tensile strength of a finished pipe at 20K is not less than 1100MPa, and the elongation after fracture is not less than 10%.
The preparation method of the near α type low-temperature titanium alloy pipe can be used for preparing the low-temperature titanium alloy pipe with the size specification of outer diameter phi of 10-120mm, wall thickness delta of 1-10mm and length L of 1000-8000mm, compared with the existing preparation method, the preparation method has the following beneficial technical effects:
1. the microstructure of the finished pipe prepared by the method is an equiaxial α microstructure or an equiaxial α + a small amount of flaky α microstructure, the tensile strength at room temperature of the finished pipe is not less than 600MPa, the yield strength is not less than 480MPa, the elongation after fracture is not less than 14%, the tensile strength at 20K is not less than 1100MPa, and the elongation after fracture is not less than 10%.
2. According to the preparation process of the low-temperature titanium alloy pipe provided by the method, as the finished pipe blank is subjected to high-temperature slow cooling vacuum heat treatment at the temperature of 5-25 ℃ below the phase transition point and then is subjected to cold rolling, coarse isometric α crystal grains with excellent low-temperature mechanical property are reserved in the structural state, meanwhile, the high distortion energy state of cold deformation is eliminated through the recrystallization process of high-temperature heat treatment, and the room-temperature strength and the shape of the pipe are improved through the cold deformation to a certain degree, so that the cold working property of the material is improved, and the room-temperature forming and the processing of subsequent complex structural parts can be carried out on the premise that the material meets the 20K high-performance requirement.
3. The finished pipe prepared by the method is in a medium-temperature stress relief annealing state after cold rolling, the wall thickness deviation is less than +/-10% of the nominal wall thickness, the outer diameter deviation is less than +/-0.5% of the nominal outer diameter, the influence of finished high-temperature heat treatment on the size precision, the straightness and the surface quality of the pipe in the existing preparation mode is completely eliminated, and the yield of the pipe is improved by about 30%.
The low-temperature titanium alloy pipe prepared by the method has the tensile strength of not less than 1100MPa at 20K and the elongation after fracture of not less than 10 percent; the tensile strength at room temperature is not less than 600MPa, the yield strength is not less than 480MPa, the elongation after fracture is not less than 14 percent, and the excellent matching of the mechanical property and the low-temperature property of the pipe can be realized. The method is suitable for the production process of preparing the low-temperature titanium alloy pipes with high dimensional accuracy in batches with various specifications and high efficiency.
Detailed Description
A preparation method of a near α type low-temperature titanium alloy pipe adopts a manufacturing method combining cold rolling and high-temperature heat treatment, and comprises the following specific operation steps:
(1) after surface scraping and boring treatment, the low-temperature titanium alloy tube blank is sent into a cogging mill for 1-2 times of large-deformation cogging rolling, and the pass deformation is controlled to be 35-60%;
(2) subjecting the cogging pipe to vacuum heat treatment at 650-750 ℃ for 1-2.5 hours, boring, scraping and removing oxide layers on the inner and outer surfaces to obtain a cold-rolled pipe blank;
(3) cold rolling the cold-rolled tube blank on a five-roller or three-roller finishing mill for 1-3 passes, and performing vacuum heat treatment at 650-750 ℃ in each pass to obtain a finished tube blank;
(4) carrying out vacuum heat treatment on the finished pipe blank at the temperature of 5-25 ℃ below the conversion temperature of α - β and the heat preservation time of 0.5-1 hour;
(5) and (3) carrying out cold rolling on the finished pipe blank after heat treatment for 1 pass, controlling the pass deformation to be 25-45%, and carrying out oil removal, acid pickling and vacuum heat treatment at 650-750 ℃ to obtain the finished pipe.
The invention is further described with reference to specific examples.
Example 1
Preparing TA7 low-temperature titanium alloy pipe with the specification of 85mm outer diameter and 2.5mm wall thickness (phi 85 multiplied by 2.5mm)
The phi 118 x 10mm low-temperature titanium alloy tube blank prepared by the oblique rolling perforation method is selected, and the main additive elements comprise, by mass, 4.9% of Al and 2.5% of Sn, and the α - β transition temperature of the TA7 low-temperature titanium alloy tube blank is 1010 ℃.
Scraping and repairing the outer surface of the cross-piercing tube blank, selecting a proper boring cutter according to the size of an inner hole, boring the inner surface, controlling the single-side feed amount to be 0.3-0.5mm, and ensuring the wall thickness deviation to be within 0.4 mm.
An LG120 type two-roller mill is selected to carry out first-pass cogging rolling, the rotating speed of the mill is 60-65 times/minute, the feeding amount is 3-4 mm/time, and the single-pass deformation amount is 55.9 percent, namely the rolling is carried out from phi 118 multiplied by 9.6mm to phi 95 multiplied by 5.1 mm; soaking and cleaning the cold-rolled cogging pipe in an ultrasonic cleaning tank by using a metal detergent to remove surface oil stains, cleaning the pipe by using a pickling solution (comprising 30% of nitric acid and 10% of hydrofluoric acid in a volume ratio, and the balance being water), performing heat treatment at 700 ℃/1 hour in vacuum heat treatment, then cooling the pipe to 200 ℃ along with a furnace, discharging the pipe from the furnace for air cooling, checking, scraping and repairing, and boring to remove internal and external surface defects to obtain the cold-rolled pipe blank.
The cold rolled pipe blank is subjected to cold rolling for 1 pass on an LD120 five-roller finishing mill, the rotating speed of the mill is 50-60 times/minute, the feeding amount is 1.5-2.5 mm/time, and the pass cold rolling deformation is 30.1 percent, namely the pipe blank is rolled from phi 95 multiplied by 4.8mm to phi 90 multiplied by 3.5 mm. Then the pipe is cleaned and degreased and then is subjected to vacuum heat treatment at 1000 ℃/1 hour, and the vacuum degree of a vacuum furnace is 1 multiplied by 10-1Pa-1×10-2Pa, the pressure increasing rate is less than or equal to 2.0 Pa/h, the temperature in the furnace is 935 +/-5 ℃, the initial cooling speed is less than or equal to 30 ℃/h, the blank is cooled to 500 ℃ and then taken out of the furnace along with the furnace cooling to room temperature, and a finished product tube blank is obtained.
Selecting a single pass on an LD120 five-roller finishing mill to roll the finished pipe blank with the diameter of 90 multiplied by 3.5mm to the diameter of 85 multiplied by 2.5mm, wherein the cold rolling deformation of the pass is 31.9%, the rotating speed of the mill is 50-60 times/minute, and the feeding amount is 1.5-2.5 mm/pass. After acid cleaning and oil removing, the pipe is subjected to heat treatment at 750 ℃/1 hour in vacuum heat treatment, and then is taken out of the furnace for air cooling when being cooled to 200 ℃ along with the furnace, so that a finished product pipe is obtained.
The microstructure of the finished titanium alloy pipe with the diameter of 85 multiplied by 2.5mm after heat treatment is equiaxial α + a small amount of flaky α structure, and the 20K mechanical properties of the finished pipe are that the tensile strength Rm is 1540MPa and the yield strength Rp0.21440MPa, and elongation after break A15%; the mechanical properties of the finished pipe at room temperature are as follows: tensile strength Rm 760MPa and yield strength Rp0.2710MPa, and elongation after break A17%.
Example 2
Preparing TA18 low-temperature titanium alloy pipe with the specification of 35mm of outer diameter and 1.5mm (phi 35 multiplied by 1.5mm) of wall thickness
A tube blank of phi 72 multiplied by 9mm low-temperature titanium alloy prepared by a sheath forward extrusion mode is selected, and the tube blank is mainly added with the chemical components of 3.1 percent of Al, 2.5 percent of V, α - β transformation temperature of the tube blank of TA18 low-temperature titanium alloy of 920 ℃ according to mass fraction.
Scraping and repairing the outer surface of the extruded tube blank, selecting a proper boring cutter according to the size of an inner hole to bore the inner surface, controlling the single-side feed amount to be 0.3-0.4 mm, and ensuring the wall thickness deviation to be within 0.3 mm.
An LG60 type two-roller mill is selected to perform two-pass cogging rolling, the rotating speed of the mill is 65-70 times/minute, and the feeding amount is 3-4 mm/time. The first pass deformation is 41.2 percent, namely the first pass is rolled from phi 72 multiplied by 8.7mm to phi 60 multiplied by 6 mm; soaking and cleaning the cold-rolled cogging pipe in an ultrasonic cleaning tank by using a metal detergent to remove surface oil stains, cleaning the pipe by using a pickling solution (comprising 15% of nitric acid and 5% of hydrofluoric acid in a volume ratio, and the balance being water), performing heat treatment at 750 ℃/1 hour in vacuum heat treatment, and then taking the pipe out of the furnace for air cooling when the pipe is cooled to 200 ℃ along with the furnace; then, the second cogging rolling is carried out by using the pass deformation of 40.6%, namely, the rolling is carried out from phi 60 multiplied by 6mm to phi 50 multiplied by 4.2 mm. And (3) carrying out acid pickling degreasing and vacuum heat treatment at 750 ℃/1 hour on the pipe subjected to the two-time cogging, and then inspecting, scraping, repairing and boring to remove the defects on the inner surface and the outer surface.
And (3) carrying out cold rolling on the cold-rolled pipe blank on an LD60 three-roller finishing mill for 2 passes, wherein the rotating speed of the mill is 50-60 times/minute, and the feeding amount is 2-3 mm/time. The first cold rolling deformation is 36.4 percent, namely the first cold rolling is carried out from phi 50 multiplied by 4mm to phi 42 multiplied by 3 mm; the cold rolling deformation of the second pass is 38.5 percent, namely, the second pass is rolled from phi 42 multiplied by 3mm to phi 38 multiplied by 2 mm. And carrying out 750 ℃/1 hour vacuum heat treatment on the pipe between two cold rolling passes to eliminate the processing stress. After cleaning and degreasing cold-rolled tube with diameter of 38 multiplied by 2mm, vacuum heat treatment is carried out for 900 ℃/1 hourThe vacuum degree of the vacuum furnace is 1X 10-2Pa, the pressure increasing rate is less than or equal to 2.0 Pa/h, the temperature in the furnace is 900 +/-5 ℃, the initial cooling speed is less than or equal to 30 ℃/h, the blank is cooled to 500 ℃ and then taken out of the furnace along with the furnace cooling to room temperature, and a finished product tube blank is obtained.
Selecting an LD60 three-roller finishing mill to roll the finished pipe blank with phi 38 multiplied by 2mm to phi 35 multiplied by 1.5mm in 1 pass, wherein the cold rolling deformation of the pass is 30.2%, the rotating speed of the mill is 50-60 times/minute, and the feeding amount is 1.5-2 mm/time. After acid cleaning and oil removing, the pipe is subjected to heat treatment at 750 ℃/1 hour in vacuum heat treatment, and then is taken out of the furnace for air cooling when being cooled to 200 ℃ along with the furnace, so that a finished product pipe is obtained.
The microstructure of the finished titanium alloy pipe with the diameter of 35 multiplied by 1.5mm after heat treatment is an equiaxial α microstructure, and the 20K mechanical properties of the finished pipe are that the tensile strength Rm is 1230MPa and the yield strength Rp0.21040MPa, elongation after break A12%; the mechanical properties of the finished pipe at room temperature are as follows: tensile strength Rm 635MPa and yield strength Rp0.2500MPa, and 20% elongation at break.
Claims (11)
1. A preparation method of a near α type low-temperature titanium alloy pipe is characterized by comprising the following steps:
(1) after surface scraping and boring treatment, the low-temperature titanium alloy tube blank is sent into a cogging mill for 1-2 times of large-deformation cogging rolling, and the pass deformation is controlled to be 35-60%;
(2) carrying out vacuum heat treatment on the cogging pipe at 650-750 ℃ for 1-2.5 hours, boring, scraping and removing oxide layers on the inner and outer surfaces to obtain a cold-rolled pipe blank;
(3) cold rolling the cold-rolled tube blank on a five-roller or three-roller finishing mill for 1-3 passes, and performing vacuum heat treatment at 650-750 ℃ in each pass to obtain a finished tube blank;
(4) carrying out vacuum heat treatment on the finished pipe blank at the temperature of 5-25 ℃ below the conversion temperature of α - β and the heat preservation time of 0.5-1 hour;
(5) and (3) carrying out 1-pass cold rolling on the finished pipe blank after heat treatment, controlling the pass deformation to be 25-45%, and carrying out oil removal, acid pickling and vacuum heat treatment at 650-750 ℃ to obtain the finished pipe.
2. The method for preparing the near α type low temperature titanium alloy pipe according to claim 1, wherein the low temperature titanium alloy pipe blank is a cross-rolled perforated pipe or a clad extruded pipe or a pipe machined by a forging machine.
3. The method for preparing the near α type low temperature titanium alloy pipe according to claim 1, wherein the boring is to remove inner wall defects including cracks and pits, and the deviation of the wall thickness of the pipe blank is less than 0.50 mm.
4. The method for preparing the low-temperature titanium alloy pipe close to α according to claim 1, wherein the low-temperature titanium alloy has a α - β transformation temperature of 900-1200 ℃.
5. The method for preparing the near α type low temperature titanium alloy pipe as claimed in claim 1, wherein the vacuum degree of the finished pipe blank is not less than 1 x 10 during vacuum heat treatment-1Pa, and the temperature deviation of the hearth is within +/-5 ℃.
6. The method for preparing the near α type low temperature titanium alloy pipe according to claim 1, wherein the cooling rate of the finished pipe blank is lower than 40 ℃/h when the finished pipe blank is subjected to vacuum heat treatment.
7. The method for preparing the near α type low temperature titanium alloy tube as claimed in claim 1, wherein the pickling solution comprises 21-30% nitric acid and 7-10% hydrofluoric acid by volume, and the balance water.
8. The method for preparing the near α type low temperature titanium alloy pipe according to claim 1, wherein the finished pipe specification is phi 15-120 x 1-10 mm.
9. The method for preparing the low-temperature titanium alloy pipe close to α according to claim 1, wherein the microstructure of the finished pipe is equiaxed α microstructure or equiaxed α + small amount of flaky α microstructure.
10. The method for preparing the near α type low temperature titanium alloy tube as claimed in claim 1, wherein the finished tube has room temperature tensile strength of not less than 600MPa, yield strength of not less than 480MPa, and elongation after fracture of not less than 14%.
11. The method for preparing the near α type low temperature titanium alloy tube, according to claim 1, wherein the finished tube has a tensile strength of not less than 1100MPa at 20K and an elongation after fracture of not less than 10%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110011936.0A CN110972521B (en) | 2011-07-26 | 2011-07-26 | Preparation method of near α type low-temperature titanium alloy pipe |
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| CN201110011936.0A CN110972521B (en) | 2011-07-26 | 2011-07-26 | Preparation method of near α type low-temperature titanium alloy pipe |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111014314A (en) * | 2019-11-27 | 2020-04-17 | 西安庄信新材料科技有限公司 | Titanium tube production and processing method |
| CN114713672A (en) * | 2022-05-09 | 2022-07-08 | 四川攀钢嘉德精工科技有限公司 | Continuous rolling warm-forming process for titanium plate |
-
2011
- 2011-07-26 CN CN201110011936.0A patent/CN110972521B/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111014314A (en) * | 2019-11-27 | 2020-04-17 | 西安庄信新材料科技有限公司 | Titanium tube production and processing method |
| CN114713672A (en) * | 2022-05-09 | 2022-07-08 | 四川攀钢嘉德精工科技有限公司 | Continuous rolling warm-forming process for titanium plate |
| CN114713672B (en) * | 2022-05-09 | 2024-04-12 | 四川攀钢嘉德精工科技有限公司 | Continuous rolling and warm forming process for titanium plate |
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Granted publication date: 20140305 Termination date: 20200726 |