CN115652139B - Niobium-titanium alloy precise strip and manufacturing method thereof - Google Patents
Niobium-titanium alloy precise strip and manufacturing method thereof Download PDFInfo
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- CN115652139B CN115652139B CN202211347689.6A CN202211347689A CN115652139B CN 115652139 B CN115652139 B CN 115652139B CN 202211347689 A CN202211347689 A CN 202211347689A CN 115652139 B CN115652139 B CN 115652139B
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- 229910001275 Niobium-titanium Inorganic materials 0.000 title claims abstract description 31
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 28
- 239000000956 alloy Substances 0.000 title claims abstract description 28
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 238000005097 cold rolling Methods 0.000 claims abstract description 45
- 238000005242 forging Methods 0.000 claims abstract description 43
- 238000005096 rolling process Methods 0.000 claims abstract description 37
- 238000010438 heat treatment Methods 0.000 claims abstract description 21
- 238000004381 surface treatment Methods 0.000 claims abstract description 14
- 238000005098 hot rolling Methods 0.000 claims abstract description 13
- 239000010936 titanium Substances 0.000 claims abstract description 9
- 230000007704 transition Effects 0.000 claims abstract description 5
- 238000000137 annealing Methods 0.000 claims description 24
- 238000004321 preservation Methods 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 19
- 238000005406 washing Methods 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 11
- 239000010955 niobium Substances 0.000 claims description 9
- 238000010304 firing Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 6
- 229910052758 niobium Inorganic materials 0.000 claims description 6
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 6
- 238000003723 Smelting Methods 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 238000003466 welding Methods 0.000 claims description 5
- 238000005238 degreasing Methods 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 230000003746 surface roughness Effects 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 230000005489 elastic deformation Effects 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000009966 trimming Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005482 strain hardening Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B1/00—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations
- B21B1/22—Metal-rolling methods or mills for making semi-finished products of solid or profiled cross-section; Sequence of operations in milling trains; Layout of rolling-mill plant, e.g. grouping of stands; Succession of passes or of sectional pass alternations for rolling plates, strips, bands or sheets of indefinite length
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B3/00—Rolling materials of special alloys so far as the composition of the alloy requires or permits special rolling methods or sequences ; Rolling of aluminium, copper, zinc or other non-ferrous metals
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
- B21B37/28—Control of flatness or profile during rolling of strip, sheets or plates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21B—ROLLING OF METAL
- B21B37/00—Control devices or methods specially adapted for metal-rolling mills or the work produced thereby
- B21B37/56—Elongation control
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
- C22C27/02—Alloys based on vanadium, niobium, or tantalum
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Metal Rolling (AREA)
Abstract
The invention discloses a niobium-titanium alloy precise strip and a manufacturing method thereof, wherein the niobium-titanium alloy precise strip comprises the following components in percentage by mass: 46-57% of Ti and 43-54% of Nb, wherein the thickness of the niobium-titanium alloy precise strip is less than or equal to 0.6 mm; the manufacturing method of the niobium-titanium alloy precise strip comprises the following steps: preparing a plate blank: cogging the ingot to obtain a plate blank, and forging the plate blank; and (3) slab warm rolling: heating the slab, and then performing hot rolling for a plurality of times, wherein the total processing rate is 60-80%; surface treatment: performing surface treatment on the plate blank after warm rolling to remove surface oxide skin to form a cold-rolled blank; cold rolling: and cold rolling the cold-rolled blank by using a special roller, wherein the special roller is a roller with the middle diameter and the edge diameter and smooth transition, and the coiled belt finished product is formed after cold rolling.
Description
Technical Field
The invention relates to the technical field of niobium-titanium alloy preparation, in particular to a niobium-titanium alloy precise strip and a manufacturing method thereof.
Background
The niobium-titanium alloy plate is generally rolled by a sheet type method to prepare a plate with the thickness not less than 2mm, and is mostly used for stamping or wire cutting to process a ring piece with a thinner wall thickness and is used for manufacturing a gasket connected with a superconducting accelerating cavity. The sheet material is relatively low in processing precision and surface quality requirements due to the subsequent size and surface processing. For niobium-titanium alloy strips, the rolling deformation resistance of the strip is lower than that of titanium alloy but is much higher than that of pure niobium, so that the thickness of the strip cannot be very thin during processing.
One of the applications of the niobium-titanium alloy precise strip is the key material used for preparing the low-temperature superconducting magnet, the wall thickness is required to be very thin, and the dimensional accuracy and the surface quality of the strip are also required to be higher. In the prior art, although the wall thickness of the existing niobium-titanium alloy strip reaches 0.6mm, other indexes of the existing niobium-titanium alloy strip are that the wall thickness deviation is less than or equal to +/-0.05 mm, the surface roughness is less than or equal to 0.8 mu m, and the flatness (H/L) is less than or equal to 6%, so that even if the existing niobium-titanium alloy strip is processed to be 0.6mm, the problems of surface wrapping, edge waviness, low dimensional accuracy control and the like exist.
Disclosure of Invention
In view of this, it is necessary to provide a niobium-titanium alloy precision strip and a method for producing the same.
The niobium-titanium alloy precise strip comprises the following components in percentage by mass: 46-57% of Ti, 42-53% of Nb and the balance of impurities, wherein the thickness of the niobium-titanium alloy precise strip is less than or equal to 0.6mm.
A manufacturing method of a niobium-titanium alloy precise strip comprises the following steps:
preparing a plate blank: cogging the ingot to obtain a plate blank, and forging the plate blank;
and (3) slab warm rolling: heating the slab, and then performing hot rolling for a plurality of times, wherein the total processing rate is 60-80%;
surface treatment: performing surface treatment on the plate blank after warm rolling to remove surface oxide skin to form a cold-rolled blank;
cold rolling: and cold rolling the cold-rolled blank by using a special roller, wherein the special roller is a special roller with large middle diameter, small edge diameter and smooth transition, and the cold-rolled blank is formed into a finished product.
The beneficial effects are that: the niobium-titanium strip prepared by the method of the invention has the advantages that the processing rate is controlled by slab warm rolling, the special slightly convex roller is adopted for cold rolling, and the pass deformation and the total deformation of cold rolling are further finely controlled, so that the thickness is thinner and smaller than 0.6mm, the thickness is preferably smaller than 0.09mm, the wall thickness deviation is less than or equal to +/-0.02 mm, the flatness (H/L) is less than or equal to 2%, the tensile strength is more than or equal to 460MPa, the specified non-proportional extension strength is more than or equal to 420MPa, the extension rate is more than or equal to 15%, the dimensional accuracy is high, the surface quality is good, the performance is stable, and the like, and the precision requirements for preparing the low-temperature superconducting magnet are completely met.
Detailed Description
The invention relates to a niobium-titanium alloy precise strip, which comprises the following components in percentage by mass: ti (46-57)%, C less than or equal to 0.04%, N less than or equal to 0.02%, H less than or equal to 0.0045%, O less than or equal to 0.10%, fe less than or equal to 0.010%, ta less than or equal to 0.10%, other impurity elements less than or equal to 0.03%, and the balance Nb, wherein the thickness of the precision strip of the niobium-titanium alloy is less than or equal to 0.6mm, preferably 0.12mm,0.09mm, the thickness deviation of the wall thickness is less than or equal to +/-0.02 mm (typically the thickness difference between the middle position and the edge of the strip), the surface roughness is less than or equal to 0.4 mu m, the flatness (H/L) is less than or equal to 2% (the algorithm of flatness is referred to a measuring method in GB/T3630-2017), the tensile strength is more than or equal to 460MPa, the specified non-proportion extension strength is more than or equal to 420MPa, the extension rate is more than or equal to 15%, and the structure is uniform.
The invention also provides a manufacturing method of the niobium-titanium alloy precise strip, which comprises the following steps:
preparing a plate blank: cogging the ingot to obtain a plate blank, and forging the plate blank;
and (3) slab warm rolling: heating the slab, and then performing a plurality of hot rolling, wherein the total processing rate is 60-80% (namely, the deformation of the two adjacent hot rolling is large, and coarse grains can be rolled to be fine, so that the existence of coarse and uneven grains is avoided);
surface treatment: performing surface treatment on the plate blank after warm rolling to remove surface oxide skin to form a cold-rolled blank;
cold rolling: and cold rolling the cold-rolled blank by using a special roller, wherein the special roller is a slightly convex roller with the middle diameter slightly larger than the edge diameter and in smooth transition, and the coiled belt finished product is formed after cold rolling.
Preferably, in the "slab preparation" step: firstly cogging and forging the cast ingot, wherein the cogging temperature is 1050-1150 ℃, the heat preservation is carried out for 4-6 hours, the forging ratio is 4-8, the final forging temperature is more than or equal to 800 ℃, then the slab forging is carried out, the temperature is 800-1000 ℃, the heat preservation is carried out for 1-3 hours, the forging ratio is 2-6, the final forging temperature is more than or equal to 750 ℃, the forging firing time of the slab is 2-4 firing times, and the specification of the slab is 30-40X 300-650 mm in thickness.
Preferably, the step of "preparing a slab" is also preceded by the step of preparing an ingot: pure titanium and pure niobium were mixed according to Ti: (46-57)%, nb: and (43-54)% by weight, pressing electrode blocks, welding the electrode blocks into a primary electrode, and smelting the primary electrode into a niobium-titanium cast ingot by using a 3-time vacuum consumable arc furnace.
Preferably, the temperature of the heated plate blank is 400-550 ℃, the heat preservation is carried out for 0.7-1.5 hours, then the hot rolling is carried out for 1-3 times, the pass deformation is 12-30%, the total processing rate is 60-80%, the thickness of the strip blank after the hot rolling is more than 1.2mm (namely, the deformation of the hot rolling for two adjacent times is large, coarse grains can be rolled finely, and the existence of coarse and uneven grains is avoided).
Preferably, the warm rolled slab is subjected to alkali washing and/or acid washing to remove surface oxide skin, then is subjected to water washing and cleaning, and then is subjected to surface polishing until the surface has no macroscopic defects.
Preferably, the alkaline washing adopts NaOH with the mass ratio of 85-95% and NaNO with the mass ratio of 15-5% 3 The mixed melt of (maintaining the temperature of the melt at 420-480 ℃), and the pickling adopts the volume ratio of HF: HNO (HNO) 3 ：H 2 O=5 to 10: 30-40: the balance of the mixed solution.
Preferably, in the cold rolling step, the number of cold rolling is 3 to 5, the pass deformation amount during cold rolling is 9 to 25% (deformation amount of the blank after rolling and before cold rolling between two anneals) and the total working ratio is 35 to 60% (deformation amount of the blank before cold rolling), the thickness of the strip formed after cold rolling is 0.6mm or less, the pass deformation amount and the total working ratio deformation amount are both large, the purpose is to refine the crystal grains, and the deformation amount is the deformation amount of cold rolling. The cold rolling thickness reaches 0.6mm, the pass deformation and the total processing rate are greatly influenced by the thickness of the strip, and each process has strict control requirements, otherwise, the strip is easy to crack or break during cold rolling.
Preferably, the thickness of the strip formed after cold rolling is less than 0.12mm.
Preferably, intermediate annealing is also performed by vacuum heat treatment before cold rolling.
Preferably, the degreasing treatment is performed before the vacuum annealing, the intermediate vacuum annealing must be performed between two rolling passes (one rolling pass between the initial pass rolling after annealing and the final pass rolling where the work hardening must be softened and annealed), and the final vacuum annealing treatment must be performed after the final rolling in order to regulate the mechanical properties.
Preferably, the degreasing treatment is also set after completion of one pass: the plate strip which needs to be subjected to heat treatment after cold rolling needs to be subjected to oil removal treatment, and the oil removal treatment is ultrasonic cleaning oil removal or oil removal agent cleaning.
Preferably, intermediate softening and finishing heat treatment are also provided after the degreasing treatment: the intermediate softening and the heat treatment of the finished product are both vacuum annealing heat treatment. (intermediate annealing temperature is 750-900 ℃, heat preservation is carried out for 1-3 hours, and vacuum degree is not less than 1X 10) - 1 Pa. The annealing temperature of the finished product is 300-450 ℃, the heat preservation is carried out for 1-3 hours, and the vacuum degree is not lower than 5 multiplied by 10 -2 Pa)
Preferably, the middle diameter of the special roller is slightly larger than the diameter of the middle of the edge by 0.1-0.6 mm. (by adopting special slightly convex roller for cold rolling, forming a strip with edges and middle thickness which are nearly consistent, the thickness deviation of the wall thickness of the strip is less than or equal to +/-0.02 mm)
Example 1Nb-50Ti niobium-titanium alloy strip having a thickness of 0.6mm×width of 600mm×20000mm (arbitrary length of > =20000 mm, not specifically limited)
(1) Ingot production
The pure titanium blank and the pure niobium are prepared according to the following proportion: ti:50%; nb:50%; pressing electrode blocks, welding the electrode blocks in combination with primary electrodes, and smelting by a vacuum consumable arc furnace for 3 times to obtain phi 600mm.
(2) Preparation of slabs
Coating the surface of the cast ingot, carrying out heat preservation for 6 hours at the forging cogging temperature of 1100 ℃, the forging ratio of 8, the final forging temperature of 850 ℃, the slab forging temperature of 850-900 ℃, and carrying out heat preservation for 2-3 hours (3 times of forging specifically, the heat preservation time is 3, 2.5 and 2 hours in sequence), wherein the forging ratio of 3-4 (3 times of forging specifically, the forging ratio of 4, 3.8 and 3 in sequence), the final forging temperature of 800 ℃, the slab specification of 30mm multiplied by 630mm of width of not less than 700mm, and the slab forging fire number of 3 fires.
(3) And (3) slab warm rolling: heating with 3 times of fire, the temperature is 450-500 ℃, the heat preservation is carried out for 1 hour, the total processing rate is 60-70%, and the final rolling thickness is 1.8mm.
(4) Surface treatment: the plate blank is subjected to alkali washing (the mixture ratio is 95 percent NaOH+5 percent NaNO) 3 ) And acid washing (the ratio is HF: HNO (HNO) 3 ：H 2 O=10: 40:50 And (3) carrying out surface polishing after washing and cleaning.
(5) Intermediate vacuum annealing: the annealing temperature is 800 ℃, the heat preservation is carried out for 1 hour, and the vacuum degree is not lower than 1 multiplied by 10 -1 Pa。
(6) Cold rolling: the pass deformation and the total processing rate are strictly controlled, the pass deformation is 12% -18%, and the total processing rate is 40% -50%. The working rolls with convexities (specifically 0.3-0.6 mm of 0.3, 0.4, 0.5 and 0.6mm of flat rolls) are adopted to carry out cold rolling through 2 rolling processes, and finally the working rolls are processed to the thickness of 0.6+/-0.02 mm (the thickness of 2 rolling processes is 1.0mm and 0.6mm respectively).
(7) And (3) heat treatment of a finished product: the annealing temperature of the finished product is 350 ℃, the heat preservation is carried out for 2 hours, and the vacuum degree is not lower than 5 multiplied by 10 -2 Pa, cooling along with the furnace.
(8) Finishing: trimming and rewinding the strip after annealing the finished product into a coiled finished product.
(9) And detecting the performance of the finished product. The test data are shown in Table 1.
Comparative example 1
On the basis of example 1, the control of the following steps was changed:
when the thickness of the rolled strip is reduced to about 0.6mm, problems such as surface wrapping, edge waviness (about 6% of flatness (H/L)), large wall thickness deviation (the thickness of the middle position of the strip is 0.69mm, the edge thickness is 0.59mm, and the wall thickness deviation is 0.1 mm) and the like occur, and even strip breakage occurs, so that the rolling is difficult to continue.
Because the roller and the deformed metal generate certain deformation in the rolling process, namely, the roller still generates elastic deformation although the rigidity is higher, and the rolled metal generates shaping and elastic deformation. Therefore, when flat roll rolling is used, the maximum amount of elastic deformation of the middle portion of the roll away from the fixed support point causes the reduction thickness of the middle portion of the strip to be minimized in the width direction, that is, corresponds to gravure roll rolling, and thus causes a phenomenon that the thickness deviation between the middle position and the edge position increases. In order to solve the problem, a certain convexity can be adopted to grind and polish the flat roller, and corresponding elastic deformation is just balanced in the rolling deformation process so as to change into flat roller rolling, so that the thickness deviation of the middle position and the edge position of the plate strip can be greatly reduced.
Example 2Nb-55Ti niobium-titanium alloy strip having a thickness of 0.12mm×width of 500mm×20000mm (arbitrary length of > =20000 mm, not specifically limited)
(1) Ingot production
The pure titanium blank and the pure niobium are prepared according to the following proportion: ti:55%, nb:45%; pressing electrode blocks, welding the electrode blocks in combination with primary electrodes, and smelting by a vacuum consumable arc furnace for 3 times to obtain phi 600mm.
(2) Preparation of slabs
Coating the surface of the cast ingot, wherein the forging and cogging temperature is 1100 ℃, the heat preservation is carried out for 6 hours, the forging ratio is 6, the final forging temperature is 800 ℃, the plate blank forging temperature is 900-950 ℃, the heat preservation is carried out for 2-3 hours, the forging ratio is 3-4, the final forging temperature is 750 ℃, the specification of the plate blank is 30mm thick and 530mm thick and is larger than or equal to 600mm wide, and the forging firing time of the plate blank is 3 firing times.
(3) And (3) slab warm rolling: heating with 3 times of fire, wherein the temperature is 450-500 ℃ (specifically, 480, 450 and 400 ℃ in sequence, for example) and preserving heat for 1 hour, the total processing rate is 60-75% (specifically, 75, 70 and 65 percent in sequence, for example) and the final rolling thickness is 1.25mm.
(4) Surface treatment: the plate blank is subjected to alkali washing (the proportion is 88 percent NaOH+12 percent NaNO) 3 ) And acid washing (the ratio is HF: HNO (HNO) 3 ：H 2 O=6: 32:62 And (3) carrying out surface polishing after washing and cleaning.
(5) Intermediate vacuum annealing: the annealing temperature is 750 ℃, the heat preservation is carried out for 1 hour, and the vacuum degree is not lower than 1 multiplied by 10 -1 Pa。
(6) Cold rolling: the pass processing rate and the total processing rate are strictly controlled, the pass deformation is 12% -20%, and the total processing rate is 45% -60%. And cold rolling with convexity (0.2-0.5 mm) through 3 rolling passes to obtain a finished product with a thickness of 0.12+/-0.012 mm (the thicknesses of 3 rolling passes are respectively 0.48mm, 0.22mm and 0.12 mm).
(7) And (3) heat treatment of a finished product: the annealing temperature of the finished product is 350 ℃, the heat preservation is carried out for 3 hours, and the vacuum degree is not lower than 5 multiplied by 10 -2 Pa, cooling along with the furnace.
(8) Finishing: trimming and rewinding the strip after annealing the finished product into a coiled finished product.
(9) And detecting the performance of the finished product. The test data are shown in Table 1.
Example 3 production method of Nb-47 Ti-niobium-titanium alloy strip with thickness of 0.09mm x 300mm x ≡30000mm
(1) Ingot production
The pure titanium blank and the pure niobium are prepared from the following components in parts by mass: ti:47%, nb:53%; pressing electrode blocks, welding the electrode blocks in combination with primary electrodes, and smelting the primary electrodes with phi 530mm in a 3-time vacuum consumable arc furnace.
(2) Preparation of slabs
Coating the surface of the cast ingot, wherein the forging and cogging temperature is 1150 ℃, the heat preservation is carried out for 6 hours, the forging ratio is 5, the final forging temperature is 800 ℃, the plate blank forging temperature is 850-900 ℃, the heat preservation is carried out for 1-3 hours, the forging ratio is 3-4, the final forging temperature is 750 ℃, the specification of the plate blank is that the thickness is 40mm, the width is 350mm, the X is not less than 800mm, and the forging firing time of the plate blank is 2 firing times.
(3) And (3) slab warm rolling: heating with 3 times of fire, the temperature is 450-500 ℃, the heat preservation is carried out for 1 hour, the total processing rate is 70-80%, and the final rolling thickness is 1.2mm.
(4) Surface treatment: the plate blank is subjected to alkali washing (the proportion is 85 percent NaOH+15 percent NaNO) 3 ) And acid washing (the ratio is HF: HNO (HNO) 3 ：H 2 O=10: 40:50 And (3) carrying out surface polishing after washing and cleaning.
(5) Intermediate vacuum annealing: the annealing temperature is 850 ℃, the heat preservation is carried out for 1 hour, and the vacuum degree is not lower than 1 multiplied by 10 -1 Pa。
(6) Cold rolling: the pass deformation is 12% -20% and the total working rate is 35% -60% (the cold rolling pass deformation and the total working rate are controlled in the above-mentioned interval, if too small, the shaping can not be fully exerted, and if too large, the crazing or breaking defect can easily occur). The working rolls with convexities (0.1-0.4 mm) are adopted to be processed to the thickness of 0.09+/-0.01 mm (the thickness of 4 rolling processes is respectively 0.48mm, 0.24mm, 0.14mm and 0.09 mm) after 4 rolling processes.
(7) And (3) heat treatment of a finished product: the annealing temperature of the finished product is 450 ℃, the heat preservation is carried out for 2 hours, and the vacuum degree is not lower than 5 multiplied by 10 -2 Pa, cooling along with the furnace.
(8) Finishing: trimming and rewinding the strip after annealing the finished product into a coiled finished product.
(9) Finished product performance was measured and the measured data are shown in table 1.
TABLE 1
The foregoing disclosure is illustrative of the preferred embodiments of the present invention, and is not to be construed as limiting the scope of the invention, as it is understood by those skilled in the art that all or part of the above-described embodiments may be practiced with equivalents thereof, which fall within the scope of the invention as defined by the appended claims.
Claims (12)
1. The niobium-titanium alloy precise strip is characterized by comprising the following components in percentage by mass: ti: 46-57%, C less than or equal to 0.04%, N less than or equal to 0.02%, H less than or equal to 0.0045%, O less than or equal to 0.10%, fe less than or equal to 0.010%, ta less than or equal to 0.10%, other impurity elements less than or equal to 0.03%, and the balance Nb, wherein the thickness of the niobium-titanium alloy precise strip is 0.09-0.12 mm or 0.12-0.6 mm, and the wall thickness deviation is +/-0.02 mm; the surface roughness is less than or equal to 0.4 mu m, the flatness is less than or equal to 2%, the algorithm of the flatness is referred to a measuring method of the unevenness in GB/T3630-2017, the tensile strength is more than or equal to 460MPa, the specified non-proportional extension strength is more than or equal to 420MPa, and the extension rate is more than or equal to 15%;
the niobium-titanium alloy precise strip is manufactured by adopting the following method, and specifically comprises the following steps:
preparing a plate blank: cogging the ingot to obtain a plate blank, and forging the plate blank;
and (3) slab warm rolling: heating the slab, and then performing hot rolling for a plurality of times, wherein the total processing rate is 60-80%; the temperature of the heated plate blank is 400-550 ℃, the heat preservation is carried out for 0.7-1.5 hours, then the hot rolling is carried out for 1-3 times, the pass deformation is 12-30%, the total processing rate is 60-80%, and the thickness of the strip blank after the hot rolling is more than 1.2mm;
surface treatment: performing surface treatment on the plate blank after warm rolling to remove surface oxide skin to form a cold-rolled blank;
cold rolling: cold rolling the cold-rolled blank by using a special roller, wherein the special roller is a special roller with large middle diameter, small edge diameter and smooth transition, and the cold-rolled blank is formed into a finished product; in the cold rolling step, the cold rolling times are 3 to 5 times, the pass deformation amount during cold rolling is 9 to 25 percent, and the total processing rate is 35 to 60 percent; the diameter difference between the middle diameter and the edge diameter of the special roller ranges from 0.1mm to 0.6mm.
2. The method for manufacturing the niobium-titanium alloy precision strip according to claim 1, comprising the following steps:
preparing a plate blank: cogging the ingot to obtain a plate blank, and forging the plate blank;
and (3) slab warm rolling: heating the slab, and then performing hot rolling for a plurality of times, wherein the total processing rate is 60-80%; the temperature of the heated plate blank is 400-550 ℃, the heat preservation is carried out for 0.7-1.5 hours, then the hot rolling is carried out for 1-3 times, the pass deformation is 12-30%, the total processing rate is 60-80%, and the thickness of the strip blank after the hot rolling is more than 1.2mm;
surface treatment: performing surface treatment on the plate blank after warm rolling to remove surface oxide skin to form a cold-rolled blank;
cold rolling: cold rolling the cold-rolled blank by using a special roller, wherein the special roller is a special roller with large middle diameter, small edge diameter and smooth transition, and the cold-rolled blank is formed into a finished product; in the cold rolling step, the cold rolling times are 3-5 times, the pass deformation amount during cold rolling is 9-25%, and the total processing rate is 35-60%.
3. The method for manufacturing a precision strip of titanium alloy according to claim 2, wherein:
in the "slab preparation" step: firstly cogging and forging the cast ingot, wherein the cogging temperature is 1050-1150 ℃, the heat preservation is carried out for 4-6 hours, the forging ratio is 4-8, the final forging temperature is more than or equal to 800 ℃, then the slab forging is carried out, the temperature is 800-1000 ℃, the heat preservation is carried out for 1-3 hours, the forging ratio is 2-6, the final forging temperature is more than or equal to 750 ℃, the forging firing time of the slab is 2-4 firing times, and the specification of the slab is 30-40X 300-650 mm in thickness.
4. The method for manufacturing a precision strip of titanium alloy according to claim 3, wherein: the "slab preparation" step is also preceded by the step of preparing the ingot: pure titanium and pure niobium were mixed according to Ti: 46-57%, nb: and (3) preparing 42-53% by weight, pressing electrode blocks, welding the electrode blocks in combination with one-time electrodes, and smelting the niobium-titanium cast ingot in a 3-time vacuum consumable arc furnace.
5. The method for manufacturing a precision strip of titanium alloy according to claim 2, wherein: the surface treatment is to perform alkali washing and/or acid washing on the warm rolled plate blank to remove surface oxide skin, and then to clean the plate blank by water washing.
6. The method for manufacturing a precision strip of titanium alloy according to claim 5, wherein: the alkaline washing adopts NaOH with the mass ratio of 85-95% and NaNO with the mass ratio of 15-5% 3 The mixed liquor of (1) is pickled by adopting the following components in percentage by mass: HNO (HNO) 3 ：H 2 O=5 to 10: 30-40: the balance of the mixed solution.
7. The method for manufacturing a precision strip of titanium alloy according to claim 2, wherein: the thickness of the strip formed after cold rolling is 0.12mm or less.
8. The method for manufacturing a precision strip of titanium alloy according to claim 2, wherein: the thickness of the strip formed after cold rolling is 0.09mm or less.
9. The method for manufacturing a precision strip of titanium alloy according to claim 2, wherein: intermediate annealing is also performed by vacuum heat treatment before cold rolling.
10. The method for manufacturing a precision strip of titanium alloy according to claim 2, wherein: deoiling treatment and intermediate vacuum annealing are carried out between the two cold rolling, and finished product vacuum annealing treatment is carried out after the rolling of the finished product.
11. The method for manufacturing a precision strip of titanium alloy according to claim 2, wherein: oil removal treatment is also provided after cold rolling: the strip material which needs to be subjected to heat treatment after cold rolling needs to be subjected to oil removal treatment, and the oil removal treatment is ultrasonic cleaning oil removal or oil removal agent cleaning.
12. The method for manufacturing a precision strip of titanium alloy according to claim 2, wherein: intermediate softening and finished product heat treatment are also arranged after the degreasing treatment: the intermediate softening and the heat treatment of the finished product are both vacuum annealing heat treatment.
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| PCT/CN2023/128464 WO2024093998A1 (en) | 2022-10-31 | 2023-10-31 | Niobium-titanium alloy precision strip and manufacturing method therefor |
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