CN116791016B - Method for eliminating titanium-rich segregation of as-cast Nb47Ti alloy by combining multidirectional forging with heat treatment - Google Patents
Method for eliminating titanium-rich segregation of as-cast Nb47Ti alloy by combining multidirectional forging with heat treatment Download PDFInfo
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- CN116791016B CN116791016B CN202310823400.1A CN202310823400A CN116791016B CN 116791016 B CN116791016 B CN 116791016B CN 202310823400 A CN202310823400 A CN 202310823400A CN 116791016 B CN116791016 B CN 116791016B
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 57
- 239000000956 alloy Substances 0.000 title claims abstract description 57
- 239000010936 titanium Substances 0.000 title claims abstract description 46
- 238000010274 multidirectional forging Methods 0.000 title claims abstract description 38
- 238000005204 segregation Methods 0.000 title claims abstract description 38
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 32
- 238000010438 heat treatment Methods 0.000 title claims abstract description 27
- 238000005242 forging Methods 0.000 claims abstract description 28
- 238000000137 annealing Methods 0.000 claims abstract description 17
- 238000009792 diffusion process Methods 0.000 claims abstract description 17
- 230000008030 elimination Effects 0.000 claims abstract description 4
- 238000003379 elimination reaction Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 11
- 239000006104 solid solution Substances 0.000 claims description 4
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 230000008569 process Effects 0.000 description 8
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 229910001275 Niobium-titanium Inorganic materials 0.000 description 6
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000010494 dissociation reaction Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000005336 cracking Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005593 dissociations Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
Classifications
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
- B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
-
- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D9/00—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor
- C21D9/0081—Heat treatment, e.g. annealing, hardening, quenching or tempering, adapted for particular articles; Furnaces therefor for slabs; for billets
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Forging (AREA)
Abstract
A method for eliminating titanium-rich segregation of an as-cast Nb47Ti alloy by multi-directional forging in combination with heat treatment, comprising: preparing an as-cast Nb47Ti alloy blank, and processing the as-cast Nb47Ti alloy into a rectangular blank; short-time high-temperature diffusion annealing the blank, and diffusion annealing the blank at high temperature; forging a blank by using a medium Wen Duoxiang forging method, and performing medium-temperature multidirectional forging on the blank subjected to high-temperature diffusion annealing; and (3) carrying out solution treatment on the blank, and placing the blank subjected to multidirectional forging into a heat treatment furnace for solution treatment to complete elimination of titanium-rich segregation. The invention solves the problems that the Nb47Ti alloy produced by the traditional method has poor plasticity caused by titanium-rich segregation, and is difficult to prepare the subsequent superconducting core wire material, successfully prepares the homogenized Nb47Ti alloy blank, and remarkably improves the plasticity and the fracture elongation of the blank.
Description
Technical Field
The invention relates to a process method for realizing homogenization of an as-cast Nb47Ti alloy, in particular to a method for eliminating titanium-rich segregation of the as-cast Nb47Ti alloy by combining multidirectional forging with heat treatment.
Background
The niobium-titanium alloy has the advantages of medium-low magnetic field superconducting performance, excellent mechanical performance and processing performance, lower cost and the like, is the only superconducting material with good plasticity in all superconducting materials at present, and has the widest application range in low-temperature superconducting materials. The Nb47Ti alloy is the most widely used alloy in the binary niobium-titanium alloy, and the main production countries are the United states and China at present. The united states Huachang corporation monopolizes most of the supply by means of high quality Nb47Ti superconducting material, which can firmly occupy the root cause of monopolized supply, is that the composition of Nb47Ti alloy bars produced and sold by the same is highly uniform, which ensures that Nb47Ti alloy bars can be processed into extremely fine core wires (< 5 μm). The Nb47Ti superconducting material can be produced in batches by two enterprises of China only including China Ningxia eastern group Co., ltd and western superconducting material science and technology Co., ltd, but the produced material often has the problem of titanium-rich segregation, so that the Nb47Ti core wire is difficult to process to be below 100 mu m.
The titanium-rich segregation is the most difficult problem to solve in preparing high-homogeneity niobium-titanium alloy, and is mainly derived from the solidification process of vacuum consumable smelting, so that the preparation and application of the subsequent superconducting wire are greatly influenced. On one hand, the titanium-rich segregation can reduce the plasticity of the niobium-titanium alloy, lead to the breakage of the core wire in the drawing process, and also can lead the core wire to generate uneven deformation, so that the superconducting performance does not reach the standard. In addition, the titanium-rich segregation may also cause the critical current density of the superconducting wire to be reduced, thereby causing the superconducting magnet to quench to cause safety accidents. In the design of the future designed magnet, the diameter of a single core wire is only about 2 mu m, and higher requirements are put on the uniformity of niobium-titanium alloy. The negative effect of titanium-rich segregation in the niobium-titanium alloy is further amplified after the size of the core wire is greatly reduced. Therefore, as a basis for producing high-performance Nb47Ti superconducting wires and magnet materials, it is important to improve and eliminate the titanium-rich segregation of Nb47Ti alloys and to realize the production of high-homogeneity Nb47Ti alloys. The traditional method for improving the titanium-rich segregation of the as-cast Nb47Ti alloy is to heat an ingot for a long time, perform free forging deformation for multiple times, and has the advantages of long production period, high cost, unobvious titanium-rich segregation improving effect, easiness in coarse crystallization and influence on the preparation of subsequent superconducting wires.
Disclosure of Invention
The invention provides a method for eliminating titanium-rich segregation of an as-cast Nb47Ti alloy by combining multidirectional forging with heat treatment to overcome the defects of the prior art. The method solves the problems that the Nb47Ti alloy produced by the traditional method has poor plasticity caused by titanium-rich segregation, and is difficult to prepare the subsequent superconducting core wire material, successfully prepares a homogenized Nb47Ti alloy blank, and remarkably improves the plasticity of the blank.
The method for eliminating titanium-rich segregation of the as-cast Nb47Ti alloy by combining multidirectional forging with heat treatment comprises the following steps:
s1, preparing an as-cast Nb47Ti alloy blank
Processing the as-cast Nb47Ti alloy into a rectangular blank;
s2, short-time high-temperature diffusion annealing blank
Diffusion annealing the blank at a high temperature;
s3, forging blank in middle Wen Duoxiang
Forging the blank subjected to high-temperature diffusion annealing at 850-1000 ℃ for Wen Duoxiang, wherein the deformation of each pass is 40%, the initial forging temperature is 1000 ℃ and the final forging temperature is 850 ℃;
s4, solid solution treatment of the blank
Placing the blank subjected to multidirectional forging into a heat treatment furnace, and carrying out solution treatment for 4 hours at 750-900 ℃ to complete elimination of titanium-rich segregation.
Compared with the prior art, the invention has the beneficial effects that:
the invention carries out high-temperature diffusion annealing, multidirectional forging and solution treatment on the produced as-cast Nb47Ti alloy, eliminates the titanium-rich segregation existing in the as-cast Nb47Ti alloy, improves the elongation at break by 115.8% compared with the original blank, and greatly improves the subsequent plastic deformation capability of the Nb47Ti alloy. Compared with the traditional method for improving the titanium-rich segregation of the as-cast Nb47Ti alloy, the method provided by the invention has the advantages of simplicity in operation, short production period, low cost, more effectiveness and reliability, and provides a new method for solving the problems that the plasticity of the Nb47Ti alloy produced in China is poor and the subsequent preparation of the superconducting core wire is difficult due to the titanium-rich segregation.
The technical scheme of the invention is further described below with reference to the accompanying drawings and examples:
drawings
FIG. 1 is an SEM image and an analysis image of Ti element content of an original as-cast billet;
FIG. 2 is a graph of tensile stress strain of an original as-cast billet;
FIG. 3 is an SEM image of a fracture after stretching of an original as-cast billet;
FIG. 4 is a schematic diagram of a multi-directional forging process;
FIG. 5 is a pictorial view of a multi-directional forged blank;
FIG. 6 is a SEM image and a Ti element content analysis image of a blank after multi-directional forging and heat treatment;
FIG. 7 is a TEM and elemental scan at the grain boundaries of a multi-directional forged and heat treated billet;
FIG. 8 is a graph of billet tensile stress strain after multi-directional forging and heat treatment;
fig. 9 is an SEM image of a fracture after multi-directional forging and heat treatment after billet stretching.
Detailed Description
Embodiments of the technical scheme of the present invention will be described in detail below with reference to the accompanying drawings. Unless otherwise defined, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs.
The method for eliminating titanium-rich segregation of the as-cast Nb47Ti alloy by combining multidirectional forging with heat treatment comprises the following steps:
s1, preparing an as-cast Nb47Ti alloy blank
Processing the as-cast Nb47Ti alloy into a rectangular blank;
for example, as-cast Nb47Ti alloy produced at home is processed into a rectangular billet of 60mm×78mm×100mm (as shown in FIG. 4, pass in the drawing indicates forging pass, and arrow indicates forging direction). The size of the blank is determined after design, and is calculated theoretically when the size of the sample meets the requirementIn the ratio, when the strain generated by each pass of the multidirectional forging is epsilon, the size ratio of the sample can be kept unchanged before and after the forging, and the infinite multidirectional forging can be realized theoretically.
S2, short-time high-temperature diffusion annealing blank
Diffusion annealing the blank at a high temperature;
for example: the billet is subjected to high-temperature diffusion annealing at 1200 ℃ for 4 hours, diffusion annealing is performed at high temperature, the atomic activity is strong, segregation can be improved through element redistribution, but the improvement effect is limited, titanium-rich segregation of an as-cast Nb47Ti alloy can not be completely eliminated only through high-temperature diffusion annealing, and the conventional long-time high-temperature diffusion annealing is easy to cause coarse grains, so that the plasticity of the material is reduced.
S3, forging blank in middle Wen Duoxiang
Forging the blank subjected to high-temperature diffusion annealing at 850-1000 ℃ for Wen Duoxiang, wherein the deformation of each pass is 40%, the initial forging temperature is 1000 ℃ and the final forging temperature is 850 ℃;
the temperature range of 850-1000 ℃ needs to be strictly controlled, and the temperature range is obtained according to a large number of dynamic thermal simulation (gleeble) experiments. On one hand, the temperature range forging can better improve the titanium-rich segregation in the Nb47Ti alloy and can not coarsely crystallize, and on the other hand, the phase transformation can be generated to alpha phase at low temperature of the Nb47Ti alloy. The alpha phase is a finite solid solution of close-packed hexagonal structure. The introduction of the alpha phase reduces the plasticity of the billet and increases the risk of cracking of the billet during the multidirectional forging process. The billet temperature during forging cannot be lower than 850 ℃.
Further, as shown in fig. 4, the schematic diagram of the multi-directional forging process is that the first forging direction is the z-axis direction, the second forging direction is the y-axis direction, the third forging direction is the x-axis direction, and the cyclic forging is performed for 6 times according to the three directions. The blank after multidirectional forging was sized and shaped to be free of cracking, as shown in fig. 5.
S4, solid solution treatment of the blank
And placing the blank subjected to multidirectional forging into a heat treatment furnace, and performing solution treatment for 4 hours at 850 ℃ to complete elimination of titanium-rich segregation.
The blank after multidirectional forging is placed into a heat treatment furnace and subjected to solution treatment at 850 ℃ for 4 hours. The method aims to re-solutionize a small amount of alpha phase structure possibly generated in the multidirectional forging process of the blank into beta phase structure, so that the structure of the blank is kept as a single phase, and the titanium-rich segregation is improved. The technological parameters of 850 ℃ and 4 hours are derived from solution treatment experiments at 750-900 ℃, the solution treatment at 850 ℃ and 900 ℃ obviously improves the titanium-rich segregation, and the temperature is considered to be high, long-time grain growth reduces the alloy plasticity, thereby influencing the subsequent wire processing and increasing the cost. Thus, the blank was quenched in water after the solution treatment at 850℃for 4 hours.
Based on the above scheme, the structure of the original blank and the blank after multidirectional forging and heat treatment is observed, fig. 1 is a structural morphology of the as-cast alloy under a Scanning Electron Microscope (SEM) and a corresponding Ti element content analysis chart, and it can be seen that a large number of holes exist, and the reason for generating the holes is that Ti element is more active than Nb element, so that under the action of corrosive agent, the area with high Ti content is corroded first to leave the holes, and the hole area is a titanium-rich segregation area. Elemental analysis was performed to find that the Ti element content at the voids was higher than in the matrix region and that the Ti element content at the voids at the grain boundaries was higher than in the intra-grain void region, indicating that the original as-cast alloy was severely rich in segregation. Fig. 6 is a SEM image of a blank after multi-directional forging and heat treatment and a corresponding Ti element content analysis image, and the visual field hardly has any voids, which proves that Ti elements in the crystal are uniformly distributed. Fig. 7 is a graph of results of scanning grain boundaries and elements under a multi-directional forging and heat-treated blank Transmission Electron Microscope (TEM), which shows that the grain boundaries and Ti elements in the grains are uniformly distributed. The method can effectively eliminate the titanium-rich segregation of the as-cast Nb47Ti alloy.
Room temperature tensile properties were tested on the original billet and the billet after multi-directional forging and heat treatment, and fig. 2 is a tensile stress strain curve of an as-cast alloy, and the elongation at break of the alloy was 19%. Fig. 3 is an SEM image of a fracture, where it can be found that there is a significant dissociation plane, with only a small number of dimples, indicating that the fracture is a quasi-dissociation fracture. FIG. 8 is a plot of tensile stress strain for a billet after multi-directional forging and heat treatment, with an elongation at break of 41% for the alloy. Fig. 9 is an SEM image of a corresponding fracture, where there are a large number of ductile pockets, and no distinct dissociation planes, indicating the fracture transition to ductile fracture. The elongation at break of the blank after multidirectional forging and heat treatment is improved by 115.8%, which indicates that the subsequent plastic deformation capability of the alloy is greatly improved.
The present invention has been described in terms of preferred embodiments, but is not limited to the invention, and any equivalent embodiments can be made by those skilled in the art without departing from the scope of the invention, as long as the equivalent embodiments are possible using the above-described structures and technical matters.
Claims (6)
1. A method for eliminating titanium-rich segregation of an as-cast Nb47Ti alloy by combining multidirectional forging with heat treatment is characterized by comprising the following steps: comprising:
s1, preparing an as-cast Nb47Ti alloy blank
Processing the as-cast Nb47Ti alloy into a rectangular blank;
s2, short-time high-temperature diffusion annealing blank
Carrying out high-temperature diffusion annealing at 1200 ℃ for 4 hours on the blank;
s3, forging blank in middle Wen Duoxiang
Forging the blank subjected to high-temperature diffusion annealing at 850-1000 ℃ for Wen Duoxiang, wherein the deformation of each pass is 40%, the initial forging temperature is 1000 ℃ and the final forging temperature is 850 ℃;
s4, solid solution treatment of the blank
Placing the blank subjected to multidirectional forging into a heat treatment furnace, and carrying out solution treatment for 4 hours at 750-900 ℃ to complete elimination of titanium-rich segregation.
2. The method for eliminating titanium-rich segregation of an as-cast Nb47Ti alloy by combination of multidirectional forging and heat treatment according to claim 1, wherein: in the multi-directional forging, the first forging direction is the z-axis direction, the second forging direction is the y-axis direction, the third forging direction is the x-axis direction, and the cyclic forging is performed for 6 times according to the three directions.
3. The method for eliminating titanium-rich segregation of an as-cast Nb47Ti alloy by combination of multidirectional forging and heat treatment according to claim 1, wherein: solution treatment was performed at 850℃or 900℃for 4 hours.
4. The method for eliminating titanium-rich segregation of an as-cast Nb47Ti alloy by combination of multidirectional forging and heat treatment according to claim 1, wherein: the blank was subjected to a solution treatment at 850℃for 4 hours, and after the solution treatment was completed, the blank was quenched in water.
5. The method for eliminating titanium-rich segregation of an as-cast Nb47Ti alloy by combination of multidirectional forging and heat treatment according to claim 1, wherein: the elongation at break of the as-cast Nb47Ti alloy was 19%.
6. The method for eliminating titanium-rich segregation of an as-cast Nb47Ti alloy by combination of multidirectional forging and heat treatment according to claim 1, wherein: the elongation at break of the billet after multidirectional forging and heat treatment was 41%.
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| CN202310823400.1A CN116791016B (en) | 2023-07-06 | 2023-07-06 | Method for eliminating titanium-rich segregation of as-cast Nb47Ti alloy by combining multidirectional forging with heat treatment |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1178117A (en) * | 1966-01-27 | 1970-01-21 | Imp Metal Ind Kynoch Ltd | Improvements in and relating to Superconductors |
| CN107413998A (en) * | 2017-07-03 | 2017-12-01 | 西部超导材料科技股份有限公司 | A kind of preparation method of Nb47Ti alloys large scale rod bar |
| CN109536777A (en) * | 2019-01-04 | 2019-03-29 | 青海聚能钛业股份有限公司 | A kind of high-temperature titanium alloy and preparation method thereof |
| CN111188001A (en) * | 2020-03-17 | 2020-05-22 | 山东理工大学 | Method for controlling silicide characteristics of high-temperature titanium-based composite material |
| CN116121588A (en) * | 2022-11-25 | 2023-05-16 | 西安圣泰金属材料有限公司 | High-performance titanium alloy for artificial joint and preparation method thereof |
-
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- 2023-07-06 CN CN202310823400.1A patent/CN116791016B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1178117A (en) * | 1966-01-27 | 1970-01-21 | Imp Metal Ind Kynoch Ltd | Improvements in and relating to Superconductors |
| CN107413998A (en) * | 2017-07-03 | 2017-12-01 | 西部超导材料科技股份有限公司 | A kind of preparation method of Nb47Ti alloys large scale rod bar |
| CN109536777A (en) * | 2019-01-04 | 2019-03-29 | 青海聚能钛业股份有限公司 | A kind of high-temperature titanium alloy and preparation method thereof |
| CN111188001A (en) * | 2020-03-17 | 2020-05-22 | 山东理工大学 | Method for controlling silicide characteristics of high-temperature titanium-based composite material |
| CN116121588A (en) * | 2022-11-25 | 2023-05-16 | 西安圣泰金属材料有限公司 | High-performance titanium alloy for artificial joint and preparation method thereof |
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