CN118222956A - Preparation method of nitrogen-containing beta titanium alloy - Google Patents
Preparation method of nitrogen-containing beta titanium alloy Download PDFInfo
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- CN118222956A CN118222956A CN202410644712.0A CN202410644712A CN118222956A CN 118222956 A CN118222956 A CN 118222956A CN 202410644712 A CN202410644712 A CN 202410644712A CN 118222956 A CN118222956 A CN 118222956A
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- 239000000956 alloy Substances 0.000 title claims abstract description 109
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 107
- 229910001040 Beta-titanium Inorganic materials 0.000 title claims abstract description 83
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000005096 rolling process Methods 0.000 claims abstract description 149
- 238000010438 heat treatment Methods 0.000 claims abstract description 94
- 238000005242 forging Methods 0.000 claims abstract description 44
- 238000000034 method Methods 0.000 claims abstract description 32
- 238000004321 preservation Methods 0.000 claims description 43
- 238000001816 cooling Methods 0.000 claims description 38
- 230000032683 aging Effects 0.000 claims description 22
- 230000000630 rising effect Effects 0.000 claims description 16
- 238000007599 discharging Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 20
- 229910001069 Ti alloy Inorganic materials 0.000 abstract description 7
- 238000005336 cracking Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 11
- 238000005098 hot rolling Methods 0.000 description 10
- 230000009467 reduction Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000000930 thermomechanical effect Effects 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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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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- 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
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Abstract
The invention relates to the technical field of titanium alloy preparation, and provides a preparation method of nitrogen-containing beta titanium alloy, which comprises the following steps: s1) rough rolling is carried out on the nitrogen-containing beta titanium alloy forging blank to obtain a rough rolled plate; the rough rolling is rolling in the length direction or rolling in the width direction; s2) carrying out forward finish rolling on the rough rolled plate to obtain a nitrogen-containing beta titanium alloy sheet; s3) performing double heat treatment on the nitrogen-containing beta titanium alloy sheet to obtain the nitrogen-containing beta titanium alloy. The invention adopts a rolling process of rough rolling and finish rolling, effectively solves the defect of finished products such as cracking, warping and the like of the nitrogen-containing beta titanium alloy Bao Banbian part, and improves the forming rate of alloy plates; by developing a large number of heat treatment processes, the rolling orientation of the plate is eliminated, and the alloy strength and plasticity are adapted. Therefore, the performance of the product prepared by the method meets the application technical requirements, and has important significance for widening the application field of the nitrogen-containing beta titanium alloy material.
Description
Technical Field
The invention relates to the technical field of titanium alloy preparation, in particular to a preparation method of nitrogen-containing beta titanium alloy.
Background
The titanium alloy has the advantages of small density and high specific strength, and the metastable beta titanium alloy also has better formability, weldability and hardenability, and excellent heat treatment performance, and can greatly improve the strength and fracture toughness after aging treatment. In the past decades, metastable beta titanium alloys have been favored by students at home and abroad, and various brands of alloys have been developed and used.
The existing common metastable beta titanium alloy is mainly used for Ti-1023 and Ti-153 alloys in the United states on cargo hold doors and main landing gear of Boeing and empty passenger A380 aircraft, BT32 and BT22U alloys prepared by Soviet Union on various large-scale complex components of aircrafts such as figure-204, ifire-76 and the like and key bearing parts, and the novel Ti-5553 metastable beta titanium alloy which is jointly developed by Boeing company and Russian VSMPO company and is used on landing gear, fuselage skeleton structure and fasteners of the aircraft of Boeing 787 aircraft; in China, the titanium alloy is developed and started later, the technology is still immature, and for the development of application type metastable beta titanium alloy products, the simulation is mainly adopted, and the principles of multi-element strengthening under the critical Mo equivalent condition are combined by the northwest nonferrous metal institute, beijing aviation materials institute, northwest industrial university and other scientific colleges, so that metastable beta titanium alloys with the same grade or higher strength with Ti-5553, such as TB19, TB20, TB17 and Ti-7333 alloys, are developed. The metastable beta titanium alloy has low heat conductivity and poor heat stability, the size of large grains of the prepared as-cast alloy can reach several millimeters, and the large grains in the structure cannot be completely crushed only by forging heat processing treatment, so that the method is not beneficial to improving the mechanical property of the alloy and widening the application field of products, and has no substantial significance for realizing engineering application of the metastable beta titanium alloy.
Ti-4.2Al-3.9V-6.2Cr-5.2Mo-1.4Fe-0.9Zr-0.25Si-0.36N is a novel nitrogen-containing high-strength metastable beta titanium alloy, and after the alloy ingot is forged, the condition that large grains in the structure are not completely broken exists, so that the subsequent development of products is limited.
The Chinese patent application with publication number of CN109554650A discloses a heat treatment process of high-strength beta titanium alloy, which mainly comprises the steps of carrying out solution aging treatment on beta titanium alloy forgings with different Mo equivalent weights, improving the strength of the titanium alloy and maintaining good plastic property; the Chinese patent application with publication number of CN116536602A discloses a tissue performance regulation method for high-strength and toughness matching of near-beta titanium alloy, which is used for improving the technical problem of high-strength and toughness matching of the alloy by carrying out solution aging treatment after carrying out three-fire free forging treatment on a beta titanium alloy cast ingot. The two inventions mainly adopt a conventional preparation method, nitrogen is not introduced into the alloy, the former focuses on carrying out one-time solution aging treatment on beta titanium alloy forgings with different Mo equivalent, the heat treatment process of the alloy is not representative, the latter mainly adopts heat treatment to regulate and control the forging structure and performance of the alloy, the two processes do not consider carrying out further thermomechanical treatment on the beta titanium alloy, the heat treatment process is not largely explored, the coarse original structure of the nitrogen-containing beta titanium alloy is not effectively changed, and finally the mechanical performance of the titanium alloy is improved.
Disclosure of Invention
The application solves the technical problem of providing a preparation method of the nitrogen-containing beta titanium alloy, which can avoid the problem of cracking and warping of the edge of the nitrogen-containing beta titanium alloy, and simultaneously realizes the effects of refining the internal structure and improving the alloy strength and plasticity.
In view of the above, the application provides a preparation method of a nitrogen-containing beta titanium alloy, which comprises the following steps:
S1) rough rolling is carried out on the nitrogen-containing beta titanium alloy forging blank to obtain a rough rolled plate; the rough rolling is rolling in the length direction or rolling in the width direction;
s2) carrying out forward finish rolling on the rough rolled plate to obtain a nitrogen-containing beta titanium alloy sheet;
s3) performing double heat treatment on the nitrogen-containing beta titanium alloy sheet to obtain a nitrogen-containing beta titanium alloy;
The rough rolling specifically comprises the following steps:
when the length direction is taken as the rolling direction, slowly heating the nitrogen-containing beta titanium alloy forging blank to 400-600 ℃ along with a furnace, preserving heat for 5-10 min, rapidly heating to 850-950 ℃ and preserving heat for 20-90 min, discharging from the furnace for first rolling, and carrying out second rolling, third rolling or fourth rolling after furnace return heat preservation, wherein the furnace return heat preservation temperature is 850-950 ℃, and preserving heat for 30-40 min, so as to obtain a rough rolling plate with the thickness less than or equal to 22 mm;
and when the width direction is taken as the rolling direction, slowly heating the nitrogen-containing beta titanium alloy forging blank to 400-600 ℃ along with a furnace, preserving heat for 5-10 min, rapidly heating to 850-950 ℃ and preserving heat for 20-90 min, discharging from the furnace for first rolling, carrying out second rolling, third rolling or fourth rolling after furnace return heat preservation, and preserving heat for 30-40 min at 850-950 ℃ at the furnace return heat preservation temperature to obtain the rough rolling plate with the thickness less than or equal to 22 mm.
Preferably, the temperature rising rate of the slow temperature rising is less than or equal to 6 ℃/min, and the temperature rising rate of the fast temperature rising is more than or equal to 15 ℃/min.
Preferably, the preparation method of the nitrogen-containing beta titanium alloy forging blank specifically comprises the following steps:
Preparing a beta titanium alloy cast ingot with the nitrogen content of 0.30-0.40 wt% by adopting a three-time VCR vacuum melting method;
and forging the beta titanium alloy cast ingot, wherein the forging temperature is 800-1200 ℃, the heat preservation time is 1-5 h, and the forging mode is three upsetting and three drawing.
Preferably, the finish rolling process specifically includes:
Slowly heating the rough rolled plate to 400-700 ℃ along with a furnace, preserving heat for 10-30 min, then rapidly heating to 800-900 ℃, preserving heat for 20-50 min, and discharging from the furnace for full longitudinal and sequential rolling; the temperature rising rate of the slow heating is less than or equal to 6 ℃/min, and the temperature rising rate of the fast heating is more than or equal to 15 ℃/min.
Preferably, the double heat treatment includes solution treatment and aging treatment performed sequentially;
The temperature of the solution treatment is 840-900 ℃, the heat preservation time is 1-2 hours, and the cooling mode is water cooling;
The temperature of the aging treatment is 450-600 ℃, the heat preservation time is 2-16 h, and the cooling mode is air cooling.
Preferably, the double heat treatment includes solution treatment and aging treatment performed sequentially;
The temperature of the solution treatment is 860-900 ℃, the heat preservation time is 1-2 hours, and the cooling mode is water cooling;
the temperature of the aging treatment is 480-530 ℃, the heat preservation time is 10-12 h, and the cooling mode is air cooling.
Preferably, the double heat treatment includes solution treatment and aging treatment performed sequentially;
the temperature of the solution treatment is 860 ℃, the heat preservation time is 1h, and the cooling mode is water cooling;
the temperature of the aging treatment is 480 ℃, the heat preservation time is 12 hours, and the cooling mode is air cooling.
Preferably, the nominal composition of the nitrogen-containing beta titanium alloy forging stock is Ti-4.2Al-3.9V-6.2Cr-5.2Mo-1.4Fe-0.9Zr-0.25Si-0.36N.
The application provides a preparation method of a nitrogen-containing beta titanium alloy, which comprises the steps of firstly, rough rolling a nitrogen-containing beta titanium alloy forging blank to obtain a rough rolled plate, then, finish rolling the rough rolled plate to obtain a thin plate, and finally, carrying out dual heat treatment on the thin plate to obtain the nitrogen-containing beta titanium alloy. In the preparation method of the nitrogen-containing beta titanium alloy, the hot rolling process means combining rough rolling and hot rolling is adopted, so that the blank obtains huge deformation, the coarse original structure of the blank is changed, large grains in the structure are completely crushed, meanwhile, a heat treatment mode of double heat treatment is adopted in the heat treatment process, and the structure morphology of the material is regulated and controlled, so that excellent mechanical properties are facilitated to be obtained.
Drawings
FIG. 1 is a diagram of a finished product of a finish rolled sheet prepared in accordance with an embodiment of the present invention;
FIG. 2 is a graph of the morphology of the transverse and longitudinal microstructures of the nitrogen-containing beta titanium alloy prepared by the invention.
Detailed Description
For a further understanding of the present invention, preferred embodiments of the invention are described below in conjunction with the examples, but it should be understood that these descriptions are merely intended to illustrate further features and advantages of the invention, and are not limiting of the claims of the invention.
In view of the requirements of incomplete crushing of coarse grains in the finish forging of the nitrogen-containing beta titanium alloy and mechanical property requirements, the application provides a preparation method of the nitrogen-containing beta titanium alloy, which effectively solves the technical problem of cracking and warping of the edge of the nitrogen-containing metastable beta titanium alloy by adopting a hot rolling process of rough rolling and finish rolling, refines the internal structure of the alloy by researching and developing a heat treatment process system suitable for the new alloy, improves the strong plasticity of the alloy, and meets the application technical requirements of products. Specifically, the embodiment of the application discloses a preparation method of a nitrogen-containing beta titanium alloy, which comprises the following steps:
S1) rough rolling is carried out on the nitrogen-containing beta titanium alloy forging blank to obtain a rough rolled plate; the rough rolling is rolling in the length direction or rolling in the width direction;
s2) carrying out forward finish rolling on the rough rolled plate to obtain a nitrogen-containing beta titanium alloy sheet;
s3) performing double heat treatment on the nitrogen-containing beta titanium alloy sheet to obtain a nitrogen-containing beta titanium alloy;
The rough rolling specifically comprises the following steps:
when the length direction is taken as the rolling direction, slowly heating the nitrogen-containing beta titanium alloy forging blank to 400-600 ℃ along with a furnace, preserving heat for 5-10 min, rapidly heating to 850-950 ℃ and preserving heat for 20-90 min, discharging from the furnace for first rolling, and carrying out second rolling, third rolling or fourth rolling after furnace return heat preservation, wherein the furnace return heat preservation temperature is 850-950 ℃, and preserving heat for 30-40 min, so as to obtain a rough rolling plate with the thickness less than or equal to 22 mm;
and when the width direction is taken as the rolling direction, slowly heating the nitrogen-containing beta titanium alloy forging blank to 400-600 ℃ along with a furnace, preserving heat for 5-10 min, rapidly heating to 850-950 ℃ and preserving heat for 20-90 min, discharging from the furnace for first rolling, carrying out second rolling, third rolling or fourth rolling after furnace return heat preservation, and preserving heat for 30-40 min at 850-950 ℃ at the furnace return heat preservation temperature to obtain the rough rolling plate with the thickness less than or equal to 22 mm.
The application provides a preparation method of a nitrogen-containing beta titanium alloy plate, which aims at the preparation method of the nitrogen-containing beta titanium alloy plate, and the chemical components of the nitrogen-containing beta titanium alloy plate meet the requirements of Ti-4.2Al-3.9V-6.2Cr-5.2Mo-1.4Fe-0.9Zr-0.25Si-0.36N, and the structure of the alloy plate is regulated and controlled through a hot rolling process and a heat treatment process, so that the performance is improved.
In the step S1), firstly, rough rolling is carried out on a nitrogen-containing beta titanium alloy forging blank to obtain a rough rolled plate; in the step, the nitrogen-containing beta titanium alloy forging blank is obtained through smelting and forging, and specifically comprises the following steps:
Preparing a beta titanium alloy cast ingot with the nitrogen content of 0.30-0.40 wt% by adopting a three-time VCR vacuum melting method;
and forging the beta titanium alloy cast ingot, wherein the forging temperature is 800-1200 ℃, the heat preservation time is 1-5 h, and the forging mode is three upsetting and three drawing. In the application, the nitrogen content in the nitrogen-containing beta titanium alloy is specifically 0.36wt%.
The VCR vacuum melting is a melting mode well known to those skilled in the art, the application is not particularly limited, the forging temperature is more specifically 900-1150 ℃, and the heat preservation time is 2-4 hours. The three upsetting and three drawing steps are specifically three upsetting steps and three drawing steps so as to realize preliminary deformation of the cast ingot. After forging and cogging, the forging surface has no obvious folds and macroscopic longitudinal cracks, and the head and the tail have no cracks. Polishing is preferably performed after forging to trim the forging stock, and the forging stock is cut into block-shaped test samples with the thickness of less than or equal to 75mm, the width of less than or equal to 120mm and the length of 300-350 mm.
The rolling of the application is specifically rolling in the length direction or rolling in the width direction, specifically, the forged blank is rolled in the length direction of 300-350 mm or the width direction of less than or equal to 120mm, and the rough rolling specifically comprises: slowly heating the nitrogen-containing beta titanium alloy forging blank to 400-600 ℃ along with a furnace, preserving heat for 5-10 min, then quickly heating to 850-950 ℃, preserving heat for 20-90 min, and then carrying out furnace returning and heat preserving rolling for 2-4 times to obtain a rough rolling plate with the thickness less than or equal to 22 mm; more specifically, the method comprises the following steps:
When the length direction is taken as the rolling direction, slowly heating the nitrogen-containing beta titanium alloy forging blank to 400-600 ℃ along with a furnace, preserving heat for 5-10 min, rapidly heating to 850-950 ℃ and preserving heat for 20-90 min, discharging the blank out of the furnace for first rolling, and then carrying out second rolling, third rolling or fourth rolling, wherein the temperature of returning to the furnace is 850-950 ℃, and preserving heat for 30-40 min;
and when the width direction is taken as the rolling direction, slowly heating the nitrogen-containing beta titanium alloy forging blank to 400-600 ℃ along with a furnace, preserving heat for 5-10 min, rapidly heating to 850-950 ℃ and preserving heat for 20-90 min, discharging from the furnace for first rolling, and then carrying out second rolling, third rolling or fourth rolling, wherein the temperature of returning to the furnace is 850-950 ℃, and preserving heat for 30-40 min.
In the above-described rolling process, for example, when the longitudinal direction is used as the rolling direction, rolling may be performed once, twice, three times, or four times; each rolling can be performed by 1 pass, 2 passes, 3 passes, 4 passes or 5 passes. Similarly, when the width direction is used as the rolling direction, rolling may be performed once, twice, three times, or four times; each rolling can be performed by 1 pass, 2 passes, 3 passes, 4 passes or 5 passes.
In the specific rolling step, the temperature rising rate of the slow temperature rising is less than or equal to 6 ℃/min, and the temperature rising rate of the fast temperature rising is more than or equal to 15 ℃/min; specifically, the temperature rising rate of the slow temperature rising is 3-5 ℃/min, and the temperature rising rate of the fast temperature rising is 18-25 ℃/min. More specifically, the temperature is slowly increased to 400-500 ℃, and the temperature is kept for 6-8 min; and the temperature is quickly raised to 880-920 ℃, the temperature is kept for 60-90 min, the temperature of the return furnace is 890-900 ℃, and the temperature is kept for 20-30 min. After the last rough rolling, the rough rolled plate with the thickness less than or equal to 22mm is obtained.
Grinding and cutting the rough rolling, and then performing finish rolling to obtain a beta titanium alloy sheet with the thickness less than or equal to 8 mm; the finish rolling specifically comprises the following steps: and slowly heating the rough rolled plate to 400-700 ℃ along with a furnace, preserving heat for 10-30 min, then rapidly heating to 800-900 ℃, preserving heat for 20-50 min, and discharging and finishing. The finish rolling is full longitudinal and forward rolling, the rough rolling plate is rolled in the same rolling direction as the last fire rolling, the heating rate of slow heating is less than or equal to 6 ℃/min, and the heating rate of rapid heating is more than or equal to 15 ℃/min; specifically, the heating rate of the slow heating is 3-5 ℃/min, and the heating rate of the fast heating is 18-25 ℃/min. Specifically, the temperature is slowly raised to 500-600 ℃, the temperature is kept for 15-20 min, the temperature is rapidly raised to 820-900 ℃, and the temperature is kept for 30-40 min. In the finish rolling process, the primary finish rolling, the secondary finish rolling and the tertiary finish rolling can be performed, the number of finish rolling is not particularly limited, and the number of passes in each finish rolling process can be 1 pass, 2 passes, 3 passes and 4 passes.
The plate subjected to the deformation treatment has large deformation resistance and unstable structure, and the regulation and control of the alloy structure and performance are realized by a heat treatment process and by making a proper heat treatment process system. The heat treatment process is double heat treatment.
The double heat treatment comprises solution treatment and aging treatment which are sequentially carried out;
the temperature of the solution treatment is 840-900 ℃, the heat preservation time is 1-2 hours, and the cooling mode is water cooling; specifically, the temperature of the solution treatment is 840 ℃, 860 ℃, 880 ℃ or 900 ℃, and the heat preservation time is 1h or 2h.
The temperature of the aging treatment is 450-600 ℃, the heat preservation time is 2-16 h, and the cooling mode is air cooling; specifically, the temperature of the aging treatment is 450 ℃, 460 ℃, 470 ℃, 490 ℃, 500 ℃, 520 ℃, 540 ℃, 560 ℃, 580 ℃ or 600 ℃, and the heat preservation time is 4 hours, 8 hours, 10 hours, 12 hours, 14 hours or 16 hours.
For the heat treatment system, specifically, the temperature of the solution treatment is 860-900 ℃, the heat preservation time is 1-2 hours, and the cooling mode is water cooling; the temperature of the aging treatment is 480-530 ℃, the heat preservation time is 10-12 h, the cooling mode is air cooling, more specifically, the temperature of the solution treatment is 860 ℃, the heat preservation time is 1h, and the cooling mode is water cooling; the temperature of the aging treatment is 480 ℃, the heat preservation time is 12 hours, and the cooling mode is air cooling.
The object researched by the invention is metastable beta titanium alloy containing 0.36wt% of nitrogen, and the research content of the hot rolling process of the alloy is not yet relevant at present, and the invention adopts a special hot rolling process path and further thermomechanical treatment aiming at the novel alloy to obtain huge deformation, change a coarse original structure and completely crush large grains in the structure; the processing temperature range of the beta titanium alloy material is narrower, the deformation resistance is sensitive to the deformation temperature and the rate parameter, a reasonable heat treatment process is required to be selected to regulate the tissue morphology of the material so as to obtain excellent mechanical properties, and the titanium alloy shows better mechanical properties under the conditions of 860-900 ℃/1-2 h/WQ+480-530 ℃/10-12 h/AC heat treatment process system.
Furthermore, the invention provides a preparation method of the nitrogen-containing metastable beta titanium alloy, which simplifies the production mode, reduces the production cost, ensures the quality of alloy plates, ensures that the plates prepared by the reversing rolling method have no edge crack and warp, has good surface quality and meets the requirements of various industrial fields.
In order to further understand the present invention, the following examples are provided to illustrate the preparation method of the nitrogen-containing beta titanium alloy according to the present invention in detail, and the scope of the present invention is not limited by the following examples.
In the embodiment of the invention and comparative example, the sources of alloy samples related to a hot rolling process and a heat treatment test are the same, the chemical components are Ti-4.2Al-3.9V-6.2Cr-5.2Mo-1.4Fe-0.9Zr-0.25Si-0.36N, a 150 kg-grade beta titanium alloy cast ingot is prepared by carrying out three VAR vacuum melting, forging and cogging are carried out after the heat preservation is carried out for 3 hours at 1150 ℃, the forged surface after three upsets and three extractions are carried out has no obvious folds and macroscopic longitudinal cracks, the head and tail are not cracked, the forging stock is polished and trimmed, and a plurality of block samples with the thickness less than or equal to 75mm, the width less than or equal to 120mm and the length of 200-350 mm are cut;
When a hot rolling test is carried out, the slow and fast heating rates of the hearth are consistent in each case, namely 5 ℃/min and 15 ℃/min, and the description is omitted in the comparative example.
Example 1
The forging stock with the sample specification of 75 multiplied by 120 multiplied by 340mm is selected, and full longitudinal and forward rolling with the length direction of 340mm as the rolling direction is carried out, and the concrete steps are as follows:
(1) Rough rolling test: heating the blank to 500 ℃ at a heating rate of 5 ℃/min along with a furnace, preserving heat for 5min, heating to 880 ℃ at a heating rate of 15 ℃/min, preserving heat for 90min, discharging from the furnace, and performing 5-pass one-fire rolling, wherein the reduction of each pass is controlled to be 16-21%; when the surface temperature of the plate is reduced to 751 ℃, carrying out furnace return heat preservation for 5-pass two-fire rolling, wherein the furnace return temperature is 910 ℃, and the heat preservation is carried out for 20min, wherein the reduction of each pass is controlled to be 4-15%, and immediately placing the plate in a water tank for quenching after rolling to obtain the plate with the thickness of 19.82 mm;
(2) Finish rolling test: the rolling direction is not changed into full longitudinal and forward rolling in the length direction, the plate sample is slowly heated to 600 ℃ along with a furnace, the temperature is kept for 20min, then the temperature is quickly increased to 850 ℃, the plate sample is kept for 50min, and then the plate sample is discharged from the furnace for 5-pass one-fire rolling, wherein the rolling reduction of each pass is controlled to be 10-16%; when the surface temperature of the plate is 745 ℃, carrying out furnace return heat preservation for 850 ℃/20min once, carrying out 4-pass rolling after discharging, controlling the rolling reduction of each pass to be 8-11%, and immediately carrying out water cooling after rolling to obtain a finish rolling plate with the thickness of 6.24 mm;
(3) Heat treatment tests, single-stage, double-stage and triple-stage heat treatment tests are carried out on the plates, and specific process systems and HRC Rockwell hardness values are shown in tables 1,2 and 3.
Example 2
A forging stock with a sample specification of 75×120×340mm (length×width×height) was selected, and reversing rolling was performed with a width direction of 120mm as a rolling direction, and the specific steps were as follows:
(1) Rough rolling test: heating the blank slowly to 500 ℃ along with the furnace, preserving heat for 5min, then heating to 880 ℃ rapidly, preserving heat for 90min, and discharging from the furnace to roll with a reduction of 14% by one fire; when the surface temperature of the plate is reduced to 745 ℃, returning to 910 ℃, and carrying out 3-pass two-fire rolling after heat preservation for 20min, wherein the reduction of each pass is controlled to be 10-22%; when the surface temperature of the plate is 748 ℃, preserving the temperature of the plate at 910 ℃ for 30min, and then performing 4-pass three-fire rolling, wherein the reduction of each pass is controlled within 9-10%; when the surface temperature of the plate is 742 ℃, carrying out furnace return heat preservation for 30min at 910 ℃ and then carrying out 3-pass four-fire rolling, wherein the rolling reduction of each pass is controlled to be 11% -16%, and the plate with the thickness of 20.02mm is obtained;
(2) Finish rolling test: the rolling direction is unchanged, the plate sample is slowly heated to 600 ℃ along with the furnace, the temperature is kept for 20min, then the temperature is quickly increased to 850 ℃, the plate sample is discharged from the furnace after the temperature is kept for 50min, and the rolling is carried out by 5 times of one-fire rolling, wherein the rolling reduction of each time is controlled to be 12-18%; returning to the furnace for heat preservation under the condition of 850 ℃/20min when the surface temperature of the plate is 743 ℃, discharging, and performing 4-pass rolling, wherein the rolling reduction of each pass is controlled to be 8-9%, and immediately performing water cooling after rolling to obtain a finish rolling plate with the thickness of 6.28 mm;
(3) The heat treatment test system was the same as in example 1, and the HRC rockwell hardness values are shown in tables 1, 2 and 3.
Table 1 shows the schedule of the single stage heat treatment process in the examples
Table 2 table of data of triple heat treatment process schedule in examples
Table 3A Dual Heat treatment Process schedule data table
The pretreatment flow of the hot rolling process and the heat treatment process after hot rolling in the embodiment 1 are the same as those in the embodiment 2, and the triple heat treatment (the triple heat treatment process selects 480 ℃/16h with single-stage heat treatment HRC more than 50 to perform triple heat treatment) is compared with the single heat treatment data, so that the triple heat treatment system is not effectively used for improving the HRC Rockwell hardness value of the new alloy, and the triple heat treatment system is eliminated; meanwhile, on the basis of the step (2), the plate after finish rolling is subjected to double heat treatment, and the result shows that the double heat treatment system obviously improves the plasticity and the strength of the nitrogen-containing beta titanium alloy.
The rough rolling in the length direction in the embodiment 1 and the rolling in the width direction in the embodiment 2 have no great influence on the mechanical properties of the alloy plate by reversing rolling, and the mechanical test result is outstanding when the heat treatment system of 860 ℃/1h/WQ+480 ℃/12h/AC is adopted in each case in the invention.
FIG. 1 is a diagram of a finished product of a finish rolled sheet prepared in accordance with an embodiment of the present invention; as can be seen from FIG. 1, the plate after finish rolling in the embodiment has no cracking and warping problems, and FIG. 2 is a graph of microstructure in transverse and longitudinal directions under the conditions of a 860 ℃/1h/WQ+480 ℃/12h/AC heat treatment process system in the embodiment, and as can be seen from FIG. 2, the size of beta grains is relatively large about 4 mu m, the precipitation of secondary alpha phase is relatively large, a large amount of secondary alpha phase is distributed at the beta grain boundary, and a small amount of secondary alpha phase is distributed at the grain boundary, and a large amount of black cluster precipitates appear in the beta grains after 12h aging treatment due to the addition of N element, thereby being beneficial to improving the hardness of alloy.
The above description of the embodiments is only for aiding in the understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. The preparation method of the nitrogen-containing beta titanium alloy comprises the following steps:
S1) rough rolling is carried out on the nitrogen-containing beta titanium alloy forging blank to obtain a rough rolled plate; the rough rolling is rolling in the length direction or rolling in the width direction;
s2) carrying out forward finish rolling on the rough rolled plate to obtain a nitrogen-containing beta titanium alloy sheet;
s3) performing double heat treatment on the nitrogen-containing beta titanium alloy sheet to obtain a nitrogen-containing beta titanium alloy;
The rough rolling specifically comprises the following steps:
when the length direction is taken as the rolling direction, slowly heating the nitrogen-containing beta titanium alloy forging blank to 400-600 ℃ along with a furnace, preserving heat for 5-10 min, rapidly heating to 850-950 ℃ and preserving heat for 20-90 min, discharging from the furnace for first rolling, and carrying out second rolling, third rolling or fourth rolling after furnace return heat preservation, wherein the furnace return heat preservation temperature is 850-950 ℃, and preserving heat for 30-40 min, so as to obtain a rough rolling plate with the thickness less than or equal to 22 mm;
and when the width direction is taken as the rolling direction, slowly heating the nitrogen-containing beta titanium alloy forging blank to 400-600 ℃ along with a furnace, preserving heat for 5-10 min, rapidly heating to 850-950 ℃ and preserving heat for 20-90 min, discharging from the furnace for first rolling, carrying out second rolling, third rolling or fourth rolling after furnace return heat preservation, and preserving heat for 30-40 min at 850-950 ℃ at the furnace return heat preservation temperature to obtain the rough rolling plate with the thickness less than or equal to 22 mm.
2. The method according to claim 1, wherein the slow heating rate is not more than 6 ℃/min and the fast heating rate is not less than 15 ℃/min.
3. The preparation method of the nitrogen-containing beta titanium alloy wrought billet according to claim 1, wherein the preparation method specifically comprises the following steps:
Preparing a beta titanium alloy cast ingot with the nitrogen content of 0.30-0.40 wt% by adopting a three-time VCR vacuum melting method;
and forging the beta titanium alloy cast ingot, wherein the forging temperature is 800-1200 ℃, the heat preservation time is 1-5 h, and the forging mode is three upsetting and three drawing.
4. The method according to claim 1, wherein the finish rolling process is specifically:
Slowly heating the rough rolled plate to 400-700 ℃ along with a furnace, preserving heat for 10-30 min, then rapidly heating to 800-900 ℃, preserving heat for 20-50 min, and discharging from the furnace for full longitudinal and sequential rolling; the temperature rising rate of the slow heating is less than or equal to 6 ℃/min, and the temperature rising rate of the fast heating is more than or equal to 15 ℃/min.
5. The production method according to claim 1, wherein the double heat treatment comprises solution treatment and aging treatment performed sequentially;
The temperature of the solution treatment is 840-900 ℃, the heat preservation time is 1-2 hours, and the cooling mode is water cooling;
The temperature of the aging treatment is 450-600 ℃, the heat preservation time is 2-16 h, and the cooling mode is air cooling.
6. The production method according to claim 1, wherein the double heat treatment comprises solution treatment and aging treatment performed sequentially;
The temperature of the solution treatment is 860-900 ℃, the heat preservation time is 1-2 hours, and the cooling mode is water cooling;
the temperature of the aging treatment is 480-530 ℃, the heat preservation time is 10-12 h, and the cooling mode is air cooling.
7. The production method according to claim 1, wherein the double heat treatment comprises solution treatment and aging treatment performed sequentially;
the temperature of the solution treatment is 860 ℃, the heat preservation time is 1h, and the cooling mode is water cooling;
the temperature of the aging treatment is 480 ℃, the heat preservation time is 12 hours, and the cooling mode is air cooling.
8. The method of claim 1, wherein the nominal composition of the wrought nitrogen-containing beta titanium alloy billet is Ti-4.2 ai-3.9V-6.2 Cr-5.2Mo-1.4Fe-0.9Zr-0.25Si-0.36N.
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