CN118048540A - High-strength niobium alloy bar and preparation method thereof - Google Patents
High-strength niobium alloy bar and preparation method thereof Download PDFInfo
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- 229910001257 Nb alloy Inorganic materials 0.000 title claims abstract description 97
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000001125 extrusion Methods 0.000 claims abstract description 41
- 238000010438 heat treatment Methods 0.000 claims abstract description 33
- 238000005096 rolling process Methods 0.000 claims abstract description 27
- 238000003723 Smelting Methods 0.000 claims abstract description 23
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000010959 steel Substances 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 15
- 238000005520 cutting process Methods 0.000 claims abstract description 15
- 238000004806 packaging method and process Methods 0.000 claims abstract description 15
- 238000001953 recrystallisation Methods 0.000 claims abstract description 9
- 239000011148 porous material Substances 0.000 claims description 18
- 238000004321 preservation Methods 0.000 claims description 18
- 239000010935 stainless steel Substances 0.000 claims description 17
- 229910001220 stainless steel Inorganic materials 0.000 claims description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- OKFDYFMLUFWESA-UHFFFAOYSA-N [Zr].[Nb].[Mo].[W] Chemical compound [Zr].[Nb].[Mo].[W] OKFDYFMLUFWESA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000005266 casting Methods 0.000 claims description 6
- 238000005098 hot rolling Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000010955 niobium Substances 0.000 claims description 6
- 238000003466 welding Methods 0.000 claims description 6
- 229910052750 molybdenum Inorganic materials 0.000 claims description 5
- 229910052721 tungsten Inorganic materials 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000005538 encapsulation Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000003912 environmental pollution Methods 0.000 abstract description 4
- 238000005253 cladding Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 9
- 238000004381 surface treatment Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000005242 forging Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a high-strength niobium alloy bar and a preparation method thereof, wherein the method comprises the following steps: 1. smelting by a vacuum consumable arc furnace to obtain a niobium alloy cast ingot and sawing an ingot riser; 2. packaging the niobium alloy cast ingot in a wrapping way, and adding steel pads at the head and the tail; 3. extruding and cogging to obtain a rod blank and cutting off a shrinkage tail; 4. heating and preserving heat, rolling to obtain a rolled bar, and straightening; 5. and (5) carrying out recrystallization annealing heat treatment after sawing and turning to obtain the niobium alloy bar. The invention adopts the process of cladding extrusion combined with multi-fire rolling, promotes the full deformation of the niobium alloy cast ingot, obviously refines the grain size of the niobium alloy cast ingot tissue, improves the tissue performance of the niobium alloy cast ingot, obtains the high-strength niobium alloy bar with large specification, uniform tissue and fine grain, improves the yield and the production efficiency of the niobium alloy bar, reduces the environmental pollution, saves the preparation cost, and is suitable for the aerospace field.
Description
Technical Field
The invention belongs to the technical field of nonferrous metal material processing, and particularly relates to a high-strength niobium alloy bar and a preparation method thereof.
Background
The high-speed development of aerospace and space technologies in China puts higher and higher requirements on the performances of refractory metal materials. For example, the structural materials in the projects of China such as lunar climbing, deep space exploration and the like not only need very high-temperature strength and excellent processability, but also bring new requirements for large specification and light weight of the materials. Compared with tungsten, molybdenum, tantalum and other alloys, the niobium alloy has small density, good economic applicability and excellent processability, becomes a first-choice material used in a high-temperature environment, is generally used for high-temperature resistant structural members of aeroengines and satellite attitude regulator nozzles, and is an important raw material for spacecrafts. The niobium alloy is usually added with high-melting-point metal elements such as tungsten, molybdenum and the like, plays roles of dispersion strengthening and solid solution strengthening, can obviously improve the high Wen Xin energy of the material, but also increases the crack sensitivity of the alloy, increases the cogging deformation difficulty, and easily generates uneven tissues to influence the final use and the processing and forming of the material.
The main production mode of the large-specification niobium alloy bar is three-time arc furnace smelting, extrusion and multi-fire forging, and the working procedures are long, the surface of the material has many cracks, multiple passes of grinding and acid washing are needed, so that the problems of low bar yield and higher manufacturing cost are caused, and the acid washing also causes environmental pollution. Patent application number 201610607717.1 discloses a production process of 30% Ti+3% Al+4.5W% +1.1% Zr+0.5% Mo niobium alloy bar, and the low-density niobium alloy bar is obtained through smelting, hot isostatic pressing, extrusion and forging, and the method does not have a clear and environment-friendly low-cost preparation technology of extrusion and rolling.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a high-strength niobium alloy bar material aiming at the defects of the prior art. The method adopts the process of cladding extrusion combined with multi-fire rolling, promotes the full deformation of the niobium alloy ingot, obviously refines the grain size of the niobium alloy ingot tissue, improves the tissue performance of the niobium alloy ingot tissue, and obtains the high-strength niobium alloy bar with large specification, uniform tissue and fine grain, thereby not only improving the yield and the production efficiency of the niobium alloy bar, but also reducing the environmental pollution, saving the preparation cost and solving the problems of long processing period, poor bar quality, low yield and environmental pollution of the traditional niobium alloy bar preparation method.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the high-strength niobium alloy bar is characterized by comprising the following steps of:
step one, ingot casting smelting: according to the mass percentage composition of the target product niobium alloy bar: 3 to 4 percent of W, 2.8 to 3.8 percent of Zr, 1 to 3 percent of Mo, 0.01 to 0.05 percent of C and the balance of Nb and unavoidable impurities, selecting a niobium-tungsten-molybdenum-zirconium strip to prepare a consumable electrode by adopting vacuum argon arc welding, then smelting the consumable electrode by adopting a three-time vacuum consumable arc furnace to obtain a niobium alloy cast ingot, sawing an ingot riser and removing surface pores and surface oxide skin;
Step two, packaging the package: adopting a stainless steel ladle sleeve to encapsulate the niobium alloy ingot with the surface pores and the surface oxide skin removed in the first step, and respectively adding a steel pad at the head and the tail of the ingot, and encapsulating the ingot in the stainless steel ladle sleeve to obtain a ladle encapsulation ingot blank;
Step three, extruding the ingot blank: extruding and cogging the sheath packaging ingot blank obtained in the second step to obtain a rod blank, and cutting off the tail of the rod blank;
Step four, rolling a bar blank: placing the rod blank subjected to tail cutting in the third step into a resistance furnace for heating and heat preservation, and then rolling for 1 fire or 2 fire on a hot rolling mill to obtain a rolled bar, and carrying out the rest Wen Jiaozhi; the diameter of the rolled bar is 3 mm-5 mm larger than that of the niobium alloy bar as a target product;
Fifth, vacuum heat treatment: sawing the rolled bar subjected to residual temperature straightening in the fourth step, turning to a target size, and then carrying out recrystallization annealing heat treatment by adopting a vacuum heat treatment furnace to obtain a niobium alloy bar; the niobium alloy bar has yield strength of more than 330MPa, tensile strength of more than 460MPa, elongation of more than 30%, reduction of area of more than 70%, uniform structure, fine grains and extremely poor grain size controlled within 2 levels.
The preparation method of the high-strength niobium alloy bar is characterized in that a 1T vacuum consumable arc furnace is adopted for three-time vacuum consumable arc furnace smelting in the first step, the vacuum degree is less than 0.3Pa, the stable smelting current is 10000A-12000A, and the dimension diameter multiplied by the height of the niobium alloy cast ingot is phi 330mm multiplied by 1000mm.
The preparation method of the high-strength niobium alloy bar is characterized in that in the second step, the stainless steel ladle sleeve is made of 1Cr18Ni9Ti stainless steel, the wall thickness of the sleeve is 6mm, the diameter of the head and the tail is3 mm-5 mm larger than that of a niobium alloy cast ingot with surface pores and surface oxide skin removed, the steel pad is a Q235 steel pad, and the size diameter multiplied by the height of the steel pad is phi 330mm multiplied by 50mm.
The preparation method of the high-strength niobium alloy bar is characterized by comprising the steps of firstly placing a sheath packaging ingot blank in a box-type resistance furnace for heat preservation at 1050 ℃ for 4-5 h before extrusion cogging, and then heating to 1100-1200 ℃ for heat preservation for 1h; the extrusion ratio of the extrusion cogging is 4-4.5, the extrusion force is 2300-2400T, and the extrusion speed is 30-50 m/s.
The preparation method of the high-strength niobium alloy bar is characterized in that the heating temperature in the fourth step is 1050-1100 ℃, the heat preservation time is 2-3 h, the single-pass deformation of rolling is 16%, and the accumulated deformation of rolling is 40% -60%.
The preparation method of the high-strength niobium alloy bar is characterized in that the annealing temperature of the recrystallization annealing heat treatment in the fifth step is 980-1080 ℃, the heat preservation time is 90-120 min, and the vacuum degree of the heat preservation section is more than 5 multiplied by 10 - 5 Pa.
The preparation method of the high-strength niobium alloy bar is characterized in that the diameter of the niobium alloy bar in the fifth step is phi 55 mm-phi 120mm.
In addition, the invention also discloses a high-strength niobium alloy bar, which is characterized by being prepared by the method. The high-strength niobium alloy bar is suitable for high-temperature environments and is generally used for high-temperature-resistant structural members of aeroengines and nozzles of satellite attitude regulators.
Compared with the prior art, the invention has the following advantages:
1. Unlike traditional extrusion and multiple forging process to prepare niobium alloy bar, which has long processing period, surface oxide layer and crack, multiple grinding and acid washing to increase loss, low yield, environment friendship and other problems.
2. According to the invention, the stainless steel sleeve is adopted to package the niobium alloy cast ingot before extrusion, so that the strong oxidization phenomenon of the niobium alloy cast ingot during high-temperature heating can be effectively avoided, the yield is improved, and a steel pad is respectively added at the head and the tail, wherein the steel pad at the head effectively avoids the uneven material structure phenomenon caused by insufficient deformation of the head of the niobium alloy cast ingot after extrusion, and the steel pad at the tail avoids the yield reduction phenomenon caused by extrusion tail shrinkage, thereby being beneficial to improving the structure property of the niobium alloy bar and improving the yield of the niobium alloy bar.
3. The extrusion process adopts a heating program of firstly preserving heat for a long time at low temperature and then raising the temperature for a short time, so that the niobium alloy cast ingot packaged by the sheath is fully heated thoroughly, coarsening and growing of crystal grains in a high-temperature environment are effectively prevented, the influence on the performance of a product is avoided, and the crystal grain size of a niobium alloy cast ingot structure can be obviously thinned by adopting a large extrusion ratio, so that the comprehensive performance of a niobium alloy bar is improved, and the operation difficulty of subsequent processing is reduced.
4. According to the invention, the heating temperature and time of the rolling of the bar blank are controlled, so that the bar blank is in an optimal deformation state, and the single-pass rolling and the accumulated deformation are controlled, so that the crack sensitivity of the niobium alloy is effectively reduced, the yield is improved, the niobium alloy is fully deformed, and the tissue uniformity is optimized.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
FIG. 1 is a high-magnification microstructure of a niobium alloy bar prepared in example 1 of the present invention.
FIG. 2 is a high magnification microstructure of the niobium alloy bar prepared in example 2 of the present invention.
FIG. 3 is a high magnification microstructure of the niobium alloy bar prepared in example 3 of the present invention.
FIG. 4 is a high magnification microstructure of the niobium alloy bar prepared in example 4 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
Step one, ingot casting smelting: according to the mass percentage composition of the target product niobium alloy bar: w3%, zr 2.9%, mo 1.2%, C0.04%, and the balance Nb and unavoidable impurities, selecting a niobium-tungsten-molybdenum-zirconium strip to prepare a consumable electrode by vacuum argon arc welding, then smelting the consumable electrode by adopting a 1T vacuum consumable arc furnace for three times by adopting the vacuum consumable arc furnace, wherein the vacuum degree is less than 0.3Pa, the stable smelting current is 10000A, obtaining a niobium alloy cast ingot with the size diameter multiplied by the height phi 330mm multiplied by 1000mm, sawing and cutting an ingot riser, and removing surface pores and surface oxide skin;
Step two, packaging the package: adopting a 1Cr18Ni9Ti stainless steel ladle sleeve to package the niobium alloy cast ingot with the surface pores and the surface oxide skin removed in the first step, wherein the thickness of the sleeve is 6mm, the diameter of the head and the tail is 3mm larger than that of the niobium alloy cast ingot with the surface pores and the surface oxide skin removed, and a Q235 steel pad with the size diameter multiplied by the height phi 330mm multiplied by 50mm is respectively added at the head and the tail, and packaged in the 1Cr18Ni9Ti stainless steel ladle sleeve to obtain a package ingot blank;
Step three, extruding the ingot blank: placing the sheath packaging ingot blank obtained in the second step into a box-type resistance furnace, preserving heat for 4 hours at 1050 ℃, then raising the temperature to 1100 ℃, preserving heat for 1 hour, performing extrusion cogging, wherein the extrusion ratio adopted by the extrusion cogging is 4, the extrusion force is 2320T, the extrusion speed is 48m/s, obtaining a rod blank with the diameter of phi 165mm, and cutting off the tail of the rod blank;
Step four, rolling a bar blank: placing the rod blank subjected to tail shrinkage cutting in the third step in a resistance furnace after surface treatment, heating and preserving heat for 3 hours at 1050 ℃, then rolling on a 550 bar hot rolling mill for 1 fire time, wherein the single-pass deformation of the 1 fire time rolling is 16%, the accumulated deformation is 37%, and obtaining a rolled bar with the diameter of phi 125mm, and carrying out the rest Wen Jiaozhi;
Fifth, vacuum heat treatment: sawing the rolled bar subjected to residual temperature straightening in the fourth step, turning to a diameter of phi 120mm, and then adopting a vacuum heat treatment furnace to perform recrystallization annealing heat treatment, wherein the annealing temperature is 980 ℃, the heat preservation time is 120min, and the vacuum degree of the heat preservation section is more than 5 multiplied by 10 -5 Pa, so as to obtain the niobium alloy bar.
Example 2
The embodiment comprises the following steps:
Step one, ingot casting smelting: according to the mass percentage composition of the target product niobium alloy bar: w4%, zr 3.7%, mo 2.9%, C0.01%, the balance Nb and unavoidable impurities, selecting a niobium-tungsten-molybdenum-zirconium strip to prepare a consumable electrode by vacuum argon arc welding, then smelting the consumable electrode by adopting a 1T vacuum consumable arc furnace for three times by adopting the vacuum consumable arc furnace, wherein the vacuum degree is less than 0.3Pa, the stable smelting current is 12000A, obtaining a niobium alloy cast ingot with the size diameter multiplied by the height phi 330mm multiplied by 1000mm, sawing and cutting an ingot riser, and removing surface pores and surface oxide skin;
Step two, packaging the package: adopting a 1Cr18Ni9Ti stainless steel ladle sleeve to package the niobium alloy cast ingot with the surface pores and the surface oxide skin removed in the first step, wherein the thickness of the sleeve is 6mm, the diameter of the head and the tail is 5mm larger than that of the niobium alloy cast ingot with the surface pores and the surface oxide skin removed, and a Q235 steel pad with the size diameter multiplied by the height phi 330mm multiplied by 50mm is respectively added at the head and the tail, and packaged in the 1Cr18Ni9Ti stainless steel ladle sleeve to obtain a package ingot blank;
Step three, extruding the ingot blank: placing the packaging ingot blank obtained in the second step into a box-type resistance furnace, preserving heat for 4 hours at 1050 ℃, then raising the temperature to 1150 ℃, preserving heat for 1 hour, performing extrusion cogging, wherein the extrusion ratio of the extrusion cogging is 4.5, the extrusion force is 2380T, the extrusion speed is 31m/s, obtaining a bar blank with the diameter of phi 155mm, and cutting off the tail of the bar blank;
Step four, rolling a bar blank: placing the rod blank subjected to tail reduction by cutting in the third step in a resistance furnace after surface treatment, heating and preserving heat for 2 hours at 1100 ℃, then rolling on a 550 bar hot rolling mill for 1 fire time, wherein the single-pass deformation of the 1 fire time rolling is 16%, the accumulated deformation is 60%, and a rolled bar with the diameter phi 95mm is obtained and subjected to the rest Wen Jiaozhi;
fifth, vacuum heat treatment: sawing the rolled bar subjected to residual temperature straightening in the fourth step, turning to a diameter phi 90mm, and then adopting a vacuum heat treatment furnace to perform recrystallization annealing heat treatment, wherein the annealing temperature is 1080 ℃, the heat preservation time is 120min, and the vacuum degree of the heat preservation section is more than 5 multiplied by 10 -5 Pa, so as to obtain the niobium alloy bar.
Example 3
The embodiment comprises the following steps:
Step one, ingot casting smelting: according to the mass percentage composition of the target product niobium alloy bar: w3%, zr 2.9%, mo 1.2%, C0.04%, and the balance Nb and unavoidable impurities, selecting a niobium-tungsten-molybdenum-zirconium strip to prepare a consumable electrode by vacuum argon arc welding, then smelting the consumable electrode by adopting a 1T vacuum consumable arc furnace for three times by adopting the vacuum consumable arc furnace, wherein the vacuum degree is less than 0.3Pa, the stable smelting current is 10000A, obtaining a niobium alloy cast ingot with the size diameter multiplied by the height phi 330mm multiplied by 1000mm, sawing and cutting an ingot riser, and removing surface pores and surface oxide skin;
Step two, packaging the package: adopting a 1Cr18Ni9Ti stainless steel ladle sleeve to package the niobium alloy cast ingot with the surface pores and the surface oxide skin removed in the first step, wherein the thickness of the sleeve is 6mm, the diameter of the head and the tail is 3mm larger than that of the niobium alloy cast ingot with the surface pores and the surface oxide skin removed, and a Q235 steel pad with the size diameter multiplied by the height phi 330mm multiplied by 50mm is respectively added at the head and the tail, and packaged in the 1Cr18Ni9Ti stainless steel ladle sleeve to obtain a package ingot blank;
step three, extruding the ingot blank: placing the sheath packaging ingot blank obtained in the second step into a box-type resistance furnace, preserving heat for 5 hours at 1050 ℃, then raising the temperature to 1200 ℃, preserving heat for 1 hour, performing extrusion cogging, wherein the extrusion ratio adopted by the extrusion cogging is 4, the extrusion force is 2310T, the extrusion speed is 45m/s, obtaining a rod blank with the diameter of phi 165mm, and cutting off the tail of the rod blank;
Step four, rolling a bar blank: placing the rod blank subjected to tail reduction in the third step after surface treatment in a resistance furnace, heating and preserving heat for 3 hours at 1050 ℃, then rolling the rod blank on a 550 bar hot rolling mill for 2 times, wherein the single-pass deformation of the 2 times is 16%, the accumulated deformation of the first time is 60%, the accumulated deformation of the second time is 58%, the rolled bar with the diameter phi of 65mm is obtained, and the rest Wen Jiaozhi is carried out;
Fifth, vacuum heat treatment: sawing the rolled bar subjected to residual temperature straightening in the fourth step, turning to a diameter of phi 60mm, and then adopting a vacuum heat treatment furnace to perform recrystallization annealing heat treatment, wherein the annealing temperature is 1000 ℃, the heat preservation time is 90min, and the vacuum degree of the heat preservation section is more than 5 multiplied by 10 -5 Pa, so as to obtain the niobium alloy bar.
Example 4
The embodiment comprises the following steps:
Step one, ingot casting smelting: according to the mass percentage composition of the target product niobium alloy bar: w4%, zr 3.7%, mo 2.9%, C0.01%, the balance Nb and unavoidable impurities, selecting a niobium-tungsten-molybdenum-zirconium strip to prepare a consumable electrode by vacuum argon arc welding, then smelting the consumable electrode by adopting a 1T vacuum consumable arc furnace for three times by adopting the vacuum consumable arc furnace, wherein the vacuum degree is less than 0.3Pa, the stable smelting current is 12000A, obtaining a niobium alloy cast ingot with the size diameter multiplied by the height phi 330mm multiplied by 1000mm, sawing and cutting an ingot riser, and removing surface pores and surface oxide skin;
Step two, packaging the package: adopting a 1Cr18Ni9Ti stainless steel ladle sleeve to package the niobium alloy cast ingot with the surface pores and the surface oxide skin removed in the first step, wherein the thickness of the sleeve is 6mm, the diameter of the head and the tail is 5mm larger than that of the niobium alloy cast ingot with the surface pores and the surface oxide skin removed, and a Q235 steel pad with the size diameter multiplied by the height phi 330mm multiplied by 50mm is respectively added at the head and the tail, and packaged in the 1Cr18Ni9Ti stainless steel ladle sleeve to obtain a package ingot blank;
Step three, extruding the ingot blank: placing the sheath packaging ingot blank obtained in the second step into a box-type resistance furnace, preserving heat for 5 hours at 1050 ℃, then raising the temperature to 1100 ℃, preserving heat for 1 hour, performing extrusion cogging, wherein the extrusion ratio of the extrusion cogging is 4.5, the extrusion force is 2390T, the extrusion speed is 32m/s, obtaining a bar blank with the diameter of phi 155mm, and cutting off the tail of the bar blank;
Step four, rolling a bar blank: placing the rod blank subjected to tail reduction in the third step after surface treatment in a resistance furnace, heating and preserving heat for 2 hours at 1100 ℃, then rolling the rod blank on a 550 bar hot rolling mill for 2 times, wherein the single-pass deformation of the 2 times of rolling is 16%, the accumulated deformation of the first time of rolling is 60%, the accumulated deformation of the second time of rolling is 56%, and a rolled bar with the diameter phi 58mm is obtained and subjected to the rest Wen Jiaozhi;
Fifth, vacuum heat treatment: sawing the rolled bar subjected to residual temperature straightening in the fourth step, turning to a diameter of phi 55mm, and then adopting a vacuum heat treatment furnace to perform recrystallization annealing heat treatment, wherein the annealing temperature is 1080 ℃, the heat preservation time is 90min, and the vacuum degree of the heat preservation section is more than 5 multiplied by 10 -5 Pa, so as to obtain the niobium alloy bar.
The mechanical properties and grain sizes of the niobium alloy rods prepared in examples 1 to 4 of the present invention were examined, and the results are shown in table 1 below.
TABLE 1
As is clear from Table 1, the niobium alloy bars prepared in examples 1 to 4 of the present invention had a yield strength of 330MPa or more, a tensile strength of 460MPa or more, an elongation of 30% or more, and a reduction of area of 70% or more; as can be seen from the high-power microstructure diagrams of fig. 1 to 4, the niobium alloy rods prepared in examples 1 to 4 had uniform high-power grain structure, fine grains, and had excellent batch uniformity with the extremely poor control within grade 2.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (8)
1. The preparation method of the high-strength niobium alloy bar is characterized by comprising the following steps of:
step one, ingot casting smelting: according to the mass percentage composition of the target product niobium alloy bar: 3 to 4 percent of W, 2.8 to 3.8 percent of Zr, 1 to 3 percent of Mo, 0.01 to 0.05 percent of C and the balance of Nb and unavoidable impurities, selecting a niobium-tungsten-molybdenum-zirconium strip to prepare a consumable electrode by adopting vacuum argon arc welding, then smelting the consumable electrode by adopting a three-time vacuum consumable arc furnace to obtain a niobium alloy cast ingot, sawing an ingot riser and removing surface pores and surface oxide skin;
Step two, packaging the package: adopting a stainless steel ladle sleeve to encapsulate the niobium alloy ingot with the surface pores and the surface oxide skin removed in the first step, and respectively adding a steel pad at the head and the tail of the ingot, and encapsulating the ingot in the stainless steel ladle sleeve to obtain a ladle encapsulation ingot blank;
Step three, extruding the ingot blank: extruding and cogging the sheath packaging ingot blank obtained in the second step to obtain a rod blank, and cutting off the tail of the rod blank;
Step four, rolling a bar blank: placing the rod blank subjected to tail cutting in the third step into a resistance furnace for heating and heat preservation, and then rolling for 1 fire or 2 fire on a hot rolling mill to obtain a rolled bar, and carrying out the rest Wen Jiaozhi; the diameter of the rolled bar is 3 mm-5 mm larger than that of the niobium alloy bar as a target product;
Fifth, vacuum heat treatment: sawing the rolled bar subjected to residual temperature straightening in the fourth step, turning to a target size, and then carrying out recrystallization annealing heat treatment by adopting a vacuum heat treatment furnace to obtain a niobium alloy bar; the niobium alloy bar has yield strength of more than 330MPa, tensile strength of more than 460MPa, elongation of more than 30%, reduction of area of more than 70%, uniform structure, fine grains and extremely poor grain size controlled within 2 levels.
2. The method for preparing the high-strength niobium alloy bar according to claim 1, wherein in the step one, a 1T vacuum consumable arc furnace is adopted for the three-time vacuum consumable arc furnace smelting, the vacuum degree is less than 0.3Pa, the stable smelting current is 10000-12000A, and the dimension diameter multiplied by the height of the niobium alloy cast ingot is phi 330mm multiplied by 1000mm.
3. The method for preparing the high-strength niobium alloy bar according to claim 1, wherein in the second step, the stainless steel sleeve is made of 1Cr18Ni9Ti stainless steel, the thickness of the sleeve wall is 6mm, the diameter of the head and the tail is 3 mm-5 mm larger than that of a niobium alloy cast ingot with surface pores and surface oxide skin removed, the steel pad is a Q235 steel pad, and the size diameter multiplied by the height of the steel pad is phi 330mm multiplied by 50mm.
4. The method for preparing the high-strength niobium alloy bar according to claim 1, wherein in the third step, before extrusion and cogging, a sheath packaging ingot blank is placed in a box-type resistance furnace, heat is preserved for 4-5 hours at 1050 ℃, and then the temperature is raised to 1100-1200 ℃ and is preserved for 1 hour; the extrusion ratio of the extrusion cogging is 4-4.5, the extrusion force is 2300-2400T, and the extrusion speed is 30-50 m/s.
5. The method for preparing the high-strength niobium alloy bar according to claim 1, wherein the heating temperature in the fourth step is 1050-1100 ℃, the heat preservation time is 2-3 h, the single-pass deformation amount of rolling is 16%, and the accumulated deformation amount of rolling is 40% -60%.
6. The method for preparing a high-strength niobium alloy bar according to claim 1, wherein the annealing temperature of the recrystallization annealing heat treatment in the fifth step is 980-1080 ℃, the heat preservation time is 90-120 min, and the vacuum degree of the heat preservation section is more than 5 x 10 -5 Pa.
7. The method for preparing a high-strength niobium alloy bar according to claim 1, wherein the diameter of the niobium alloy bar in the fifth step is phi 55 mm-phi 120mm.
8. A high strength niobium alloy rod produced by the method of any one of claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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