CN110580984A - Preparation method of copper-clad bronze/Nb composite rod - Google Patents
Preparation method of copper-clad bronze/Nb composite rod Download PDFInfo
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- CN110580984A CN110580984A CN201810595510.6A CN201810595510A CN110580984A CN 110580984 A CN110580984 A CN 110580984A CN 201810595510 A CN201810595510 A CN 201810595510A CN 110580984 A CN110580984 A CN 110580984A
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- H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
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Abstract
The invention provides a preparation method of a copper-clad bronze/Nb composite rod, which comprises the following steps: (1) cleaning the material; (2) putting the porous bronze ingot into a copper pipe, inserting a Nb or Nb alloy rod into the porous bronze ingot, and adding copper covers at two ends of the porous bronze ingot and sealing and welding by adopting an electron beam; (3) extruding the copper/bronze/Nb composite sheath obtained in the step (2); (4) and (4) repeatedly drawing and annealing the copper/bronze/Nb extrusion rod obtained in the step (3), and removing the copper layer on the surface in a scalping or grinding mode when the size is small to obtain the bronze/Nb composite rod. According to the invention, the copper layer with excellent processing performance is coated outside the bronze/Nb composite rod, so that the copper layer can wrap the bronze/Nb composite body inside, bronze cracking is effectively avoided, and the copper layer is removed in a peeling or grinding mode when the size is small, so that the bronze/Nb composite rod for processing the Nb3Sn composite wire by the bronze method is obtained.
Description
Technical Field
The invention belongs to the technical field of superconducting material processing, and relates to a preparation method of a bronze/Nb composite rod for a bronze Nb3Sn superconducting wire.
Background
The bronze Nb3Sn superconducting wire is one of the main materials for manufacturing high field magnets, bronze is used as a matrix, and the bronze is severely hardened by working, so that intermediate annealing is required to be repeatedly performed during the working. The Nb3Sn phase is generated in the processing process due to the excessively high annealing temperature, and the core wire is in a sausage shape, so that the critical current is reduced; the low annealing temperature can cause poor plasticity of bronze and easy longitudinal cracking, thereby the material is scrapped. Generally, a higher annealing temperature is used to improve the occurrence of cracking, but from the viewpoint of improving the performance of the bronze Nb3Sn superconducting wire, the lower the intermediate annealing temperature, the better. Meanwhile, the difference of the processing performances of bronze and Nb in the bronze/Nb complex is large, and the bronze matrix is cracked due to uneven stress distribution caused by processing, so that materials are scrapped. Therefore, the preparation method of the high-tin bronze/Nb composite rod which is not easy to crack in the processing process is found, and the cost can be effectively reduced.
Disclosure of Invention
Aiming at the technical problems that in the prior art, the difference of the processing performances of bronze and Nb in a bronze/Nb complex is large, and the stress distribution caused by processing is uneven, so that the bronze matrix is cracked, and the material is scrapped, the invention provides the preparation method of the copper-clad bronze/Nb composite rod.
The invention provides a preparation method of a copper-clad bronze/Nb composite rod, which comprises the following steps:
(1) and cleaning the copper pipe, the porous bronze ingot, the Nb or Nb alloy rod.
(2) And putting the porous bronze ingot into a copper pipe, inserting the Nb or Nb alloy rod into the porous bronze ingot, adding copper covers at two ends of the porous bronze ingot, and sealing and welding by adopting electron beams to obtain the copper/bronze/Nb composite sheath.
(3) And (3) heating the multi-core bronze/Nb sheath obtained in the step (2) and then extruding to obtain the copper/bronze/Nb extrusion rod.
(4) And (4) repeatedly drawing and annealing the copper/bronze/Nb extrusion rod obtained in the step (3), and removing a copper layer on the surface in a scalping or grinding mode when the size is small to obtain the bronze/Nb composite rod for preparing the Nb3Sn wire rod by the bronze method.
In the step (1), Sn accounts for 13.5-16.0% by mass of the porous bronze ingot, and Ti accounts for 0.2-0.4% by mass of the porous bronze ingot.
Preferably, in the porous bronze ingot obtained in step (1) of the present invention, Sn is 14.2% by mass and Ti is 0.3% by mass.
The outer diameter of the porous bronze ingot in the step (1) is phi 110 mm-phi 170mm, the number of the holes is 19 or 37, the diameter of the holes is phi 9 mm-phi 23mm, the ratio of the distance between the holes to the diameter of the holes is 0.15-0.40, and the length is 300 mm-600 m; the outer diameter of the copper pipe is phi 120 mm-phi 185mm, the inner diameter of the copper pipe is consistent with the outer diameter of the porous bronze ingot, and the length of the copper pipe is 300 mm-600 m.
Preferably, the outer diameter of the porous bronze ingot in the step (1) of the invention is phi 140mm, the number of the holes is 37, the diameter of the holes is phi 16mm, the ratio of the distance between the holes to the diameter of the holes is 0.27, and the length is 450 m; the outer diameter of the copper pipe is phi 152mm, the inner diameter of the copper pipe is consistent with the outer diameter of the porous bronze ingot, and the length of the copper pipe is 450 m.
The Nb alloy in the step (1) is an Nb-Ti rod with the mass percent of Ti of 0.5-2.0%, or an Nb-Ta rod with the mass percent of Ta of 0.5-2.0%.
Preferably, the step (1) Nb alloy of the invention is Nb-Ti rod with 1.2 mass percent of Ti or Nb-Ta rod with 1.3 mass percent of Ta.
The ratio of the sectional areas of the bronze and the Nb or Nb alloy rod in the step (1) is 2.0-3.0.
Preferably, the ratio of the cross-sectional area of the bronze to the Nb or Nb alloy rods in step (1) of the present invention is 2.5.
The specific method for cleaning in the step (1) comprises the following steps: firstly, removing oil stains on the surface by using a metal cleaner, and then cleaning the bronze material by using a nitric acid solution, wherein the volume concentration of the nitric acid solution is 25-40%; the Nb or Nb alloy rod is cleaned by adopting a mixed solution of nitric acid, hydrofluoric acid and water, and the volume concentration of each component in the mixed solution is as follows: 25-35% of nitric acid, 15-25% of hydrofluoric acid and the balance of water.
Preferably, the volume concentration of the nitric acid solution for cleaning the bronze material in the step (1) of the invention is 32.5%; the volume concentration of each component in the mixed solution of the Nb or Nb alloy rods is as follows: 30% of nitric acid, 20% of hydrofluoric acid and the balance of water.
in the step (2), the current of the electron beam sealing welding is 30-100 mA, and the vacuum degree is less than 1.0 multiplied by 10 < -2 > Pa.
Preferably, in step (2) of the present invention, the electron beam sealing current is 65mA, and the vacuum degree is 5.0X 10-3 Pa.
In the step (3), the preheating temperature of the sheath is 550-670 ℃, the heat preservation time is 2-4 h, and the extrusion ratio is 8-15.
Preferably, in step (3) of the invention, the preheating temperature of the sheath is 610 ℃, the holding time is 3h, and the extrusion ratio is 11.5.
in the invention, the copper/bronze/Nb composite rod obtained in the step (4) is subjected to intermediate annealing when the working rate of each drawing is 12-25%, the drawing speed is 5-20 m/min, and the total drawing working rate is less than or equal to 50%.
Preferably, the copper/bronze/Nb composite rod obtained in step (4) of the present invention is subjected to intermediate annealing at a drawing rate of 19% per drawing, a drawing speed of 12m/min and a total drawing rate of 50%.
In the invention, the intermediate annealing temperature in the step (4) is 400-620 ℃, and the heat preservation time is 1-3 h.
Preferably, the interannealing temperature in the step (4) of the invention is 510 ℃, and the holding time is 2 h.
In the invention, after the copper/bronze/Nb composite rod in the step (4) is processed to phi 15mm, the copper layer coated on the surface is removed by adopting a peeling or grinding mode.
The invention has the beneficial effects that:
According to the preparation method of the bronze/Nb composite rod processed by copper-clad, the copper layer with excellent processing performance is coated on the outer portion of the bronze/Nb composite rod, a wrapping effect is formed on the bronze/Nb complex in the bronze/Nb composite rod, bronze cracking is effectively avoided, the copper layer is removed in a peeling or grinding mode when the size is small, the bronze/Nb composite rod for processing the Nb3Sn composite wire by the bronze method is obtained, the obtained bronze/Nb composite rod is uniform in quality and stress distribution, and the bronze/Nb composite rod is free of cracking.
Drawings
FIG. 1 is a schematic representation of the copper/bronze/Nb composite sheath of the present invention.
1-Nb or Nb alloy rods of FIG. 1; 2-a porous bronze ingot; 3-copper tube.
Detailed Description
The following description of the embodiments of the present invention will be made in further detail with reference to fig. 1 and examples, but the method of the present invention is not limited to the following examples.
the invention provides a preparation method of a copper-clad bronze/Nb composite rod, which comprises the following steps:
(1) the method for cleaning the copper pipe, the porous bronze ingot, the Nb or Nb alloy rod comprises the following specific steps: firstly, removing oil stains on the surface by using a metal cleaner, and then cleaning the bronze material by using a nitric acid solution, wherein the volume concentration of the nitric acid solution is 25-40%; the Nb or Nb alloy rod is cleaned by adopting a mixed solution of nitric acid, hydrofluoric acid and water, and the volume concentration of each component in the mixed solution is as follows: 25-35% of nitric acid, 15-25% of hydrofluoric acid and the balance of water; the mass percent of Sn in the porous bronze ingot is 13.5-16.0%, the mass percent of Sn in the porous bronze ingot is 0.2-0.4% of Ti element, the outer diameter of the porous bronze ingot is phi 110 mm-phi 170mm, the number of holes is 19 or 37, the diameter of the holes is phi 9 mm-phi 23mm, the ratio of the distance between the holes to the diameter of the holes is 0.15-0.40, and the length of the holes is 300 mm-600 m; the outer diameter of the copper pipe is phi 120 mm-phi 185mm, the inner diameter of the copper pipe is consistent with the outer diameter of the porous bronze ingot, the length of the copper pipe is 300 mm-600 m, the Nb alloy is an Nb-Ti rod with the mass percent of Ti of 0.5% -2.0%, or is an Nb-Ta rod with the mass percent of Ta of 0.5% -2.0%, and the cross-sectional area ratio of bronze to Nb or Nb alloy rods is 2.0-3.0.
(2) Putting a porous bronze ingot into a copper pipe, inserting a Nb or Nb alloy rod into the porous bronze ingot, adding copper covers at two ends of the porous bronze ingot, and sealing and welding by adopting an electron beam to obtain a copper/bronze/Nb composite sheath, wherein the current of the electron beam sealing and welding is 30-100 mA, and the vacuum degree is less than 1.0 multiplied by 10 < -2 > Pa.
(3) And (3) heating the multi-core bronze/Nb sheath obtained in the step (2) and then extruding to obtain a copper/bronze/Nb extrusion rod, wherein the preheating temperature of the sheath is 550-670 ℃, the heat preservation time is 2-4 h, and the extrusion ratio is 8-15.
(4) and (3) repeatedly drawing and intermediate annealing the copper/bronze/Nb extrusion rod obtained in the step (3), removing a copper layer on the surface by adopting a peeling or grinding mode when the size is phi 15mm, and obtaining the bronze/Nb composite rod for preparing the Nb3Sn wire rod by the bronze method, wherein the processing rate of each drawing of the copper/bronze/Nb composite rod is 12-25%, the drawing speed is 5-20 m/min, and the intermediate annealing is carried out when the total drawing processing rate is less than or equal to 50%. The intermediate annealing temperature is 400-620 ℃, and the heat preservation time is 1-3 h. As shown in figure 1 of the specification.
The first embodiment is as follows: the invention discloses a preparation method of copper-clad bronze/Nb composite rod
The invention provides a preparation method of a copper-clad bronze/Nb composite rod, which comprises the following steps:
(1) The method for cleaning the copper pipe, the porous bronze ingot, the Nb or Nb alloy rod comprises the following specific steps: firstly, removing oil stains on the surface by using a metal cleaner, and then cleaning the bronze material by using a nitric acid solution, wherein the volume concentration of the nitric acid solution is 32.5%; the Nb or Nb alloy rod is cleaned by adopting a mixed solution of nitric acid, hydrofluoric acid and water, and the volume concentration of each component in the mixed solution is as follows: 30% of nitric acid, 20% of hydrofluoric acid and the balance of water; the mass percent of Sn in the porous bronze ingot is 14.2%, the porous bronze ingot contains 0.3% of Ti element, the outer diameter of the porous bronze ingot is phi 140mm, the number of holes is 37, the diameter of the holes is phi 16mm, the ratio of the space among the holes to the diameter of the holes is 0.27, and the length of the porous bronze ingot is 450 m; the outer diameter of the copper pipe is phi 152mm, the inner diameter of the copper pipe is consistent with the outer diameter of the porous bronze ingot, the length of the copper pipe is 450m, the Nb alloy is an Nb-Ti rod with the mass percent of Ti being 1.2%, or an Nb-Ta rod with the mass percent of Ta being 1.3%, and the sectional area ratio of the bronze to the Nb or Nb alloy rod is 2.5.
(2) putting a porous bronze ingot into a copper pipe, inserting a Nb or Nb alloy rod into the porous bronze ingot, adding copper covers at two ends of the porous bronze ingot, and sealing and welding by adopting electron beams to obtain a copper/bronze/Nb composite sheath, wherein the current of the electron beam sealing and welding is 65mA, and the vacuum degree is 5.0 multiplied by 10 < -3 > Pa.
(3) And (3) heating the multi-core bronze/Nb sheath obtained in the step (2) and then extruding to obtain a copper/bronze/Nb extrusion rod, wherein the preheating temperature of the sheath is 610 ℃, the heat preservation time is 3 hours, and the extrusion ratio is 11.5.
(4) And (3) repeatedly drawing and performing intermediate annealing on the copper/bronze/Nb extrusion rod obtained in the step (3), removing a copper layer on the surface by adopting a peeling or grinding mode when the size is phi 15mm, and obtaining the bronze/Nb composite rod for preparing the Nb3Sn wire rod by the bronze method, wherein the processing rate of each drawing of the copper/bronze/Nb composite rod is 19%, the drawing speed is 12m/min, and the intermediate annealing is performed when the total processing rate of drawing is equal to 50%. The intermediate annealing temperature is 510 ℃, and the holding time is 2 h.
Example two: the invention discloses a preparation method of copper-clad bronze/Nb composite rod
The invention provides a preparation method of a copper-clad bronze/Nb composite rod, which comprises the following steps:
(1) The method for cleaning the copper pipe, the porous bronze ingot, the Nb or Nb alloy rod comprises the following specific steps: firstly, removing oil stains on the surface by using a metal cleaner, and then cleaning the bronze material by using a nitric acid solution, wherein the volume concentration of the nitric acid solution is 40%; the Nb or Nb alloy rod is cleaned by adopting a mixed solution of nitric acid, hydrofluoric acid and water, and the volume concentration of each component in the mixed solution is as follows: 35% of nitric acid, 25% of hydrofluoric acid and the balance of water; the mass percent of Sn in the porous bronze ingot is 16.0%, the mass percent of the Sn is 0.4% of Ti element, the outer diameter of the porous bronze ingot is phi 170mm, the number of holes is 37, the diameter of the holes is phi 23mm, the ratio of the space among the holes to the diameter of the holes is 0.40, and the length of the holes is 600 m; the outer diameter of the copper pipe is phi 185mm, the inner diameter of the copper pipe is consistent with the outer diameter of the porous bronze ingot, the length of the copper pipe is 600m, the Nb alloy is an Nb-Ti rod with the mass percent of Ti of 2.0%, or an Nb-Ta rod with the mass percent of Ta of 2.0%, and the sectional area ratio of the bronze to the Nb or Nb alloy rod is 3.0.
(2) putting a porous bronze ingot into a copper pipe, inserting a Nb or Nb alloy rod into the porous bronze ingot, adding copper covers at two ends of the porous bronze ingot, and sealing and welding by adopting electron beams to obtain a copper/bronze/Nb composite sheath, wherein the current of the electron beam sealing and welding is 100mA, and the vacuum degree is 9.0 multiplied by 10 < -3 > Pa.
(3) and (3) heating the multi-core bronze/Nb sheath obtained in the step (2) and then extruding to obtain a copper/bronze/Nb extrusion rod, wherein the preheating temperature of the sheath is 670 ℃, the heat preservation time is 4h, and the extrusion ratio is 15.
(4) And (3) repeatedly drawing and performing intermediate annealing on the copper/bronze/Nb extrusion rod obtained in the step (3), removing a copper layer on the surface by adopting a peeling or grinding mode when the size is phi 15mm, and obtaining the bronze/Nb composite rod for preparing the Nb3Sn wire rod by the bronze method, wherein the machining rate of each drawing of the copper/bronze/Nb composite rod is 25%, the drawing speed is 20m/min, and the intermediate annealing is performed when the total machining rate of the drawing is equal to 40%. The intermediate annealing temperature is 620 ℃, and the heat preservation time is 3 h.
Example three: the invention discloses a preparation method of copper-clad bronze/Nb composite rod
The invention provides a preparation method of a copper-clad bronze/Nb composite rod, which comprises the following steps:
(1) The method for cleaning the copper pipe, the porous bronze ingot, the Nb or Nb alloy rod comprises the following specific steps: firstly, removing oil stains on the surface by using a metal cleaner, and then cleaning the bronze material by using a nitric acid solution, wherein the volume concentration of the nitric acid solution is 25 percent; the Nb or Nb alloy rod is cleaned by adopting a mixed solution of nitric acid, hydrofluoric acid and water, and the volume concentration of each component in the mixed solution is as follows: 25% of nitric acid, 15% of hydrofluoric acid and the balance of water; the mass percent of Sn in the porous bronze ingot is 13.5 percent, the mass percent of Sn in the porous bronze ingot is 0.2 percent of Ti element, the outer diameter of the porous bronze ingot is phi 110mmmm, the number of holes is 19, the diameter of each hole is phi 9mmmm, the ratio of the distance between the holes to the diameter of each hole is 0.15, and the length of each hole is 300 mm; the outer diameter of the copper pipe is phi 120mm, the inner diameter of the copper pipe is consistent with the outer diameter of the porous bronze ingot, the length of the copper pipe is 300mm, the Nb alloy is an Nb-Ti rod with 0.5 mass percent of Ti or an Nb-Ta rod with 0.5 mass percent of Ta, and the sectional area ratio of bronze to Nb or Nb alloy rod is 2.0.
(2) Putting a porous bronze ingot into a copper pipe, inserting a Nb or Nb alloy rod into the porous bronze ingot, adding copper covers at two ends of the porous bronze ingot, and sealing and welding by adopting electron beams to obtain a copper/bronze/Nb composite sheath, wherein the current of the electron beam sealing and welding is 30mA, and the vacuum degree is 1.0 multiplied by 10 < -2 > Pa.
(3) And (3) heating the multi-core bronze/Nb sheath obtained in the step (2) and then extruding to obtain a copper/bronze/Nb extrusion rod, wherein the preheating temperature of the sheath is 550 ℃, the heat preservation time is 2 hours, and the extrusion ratio is 8.
(4) And (3) repeatedly drawing and performing intermediate annealing on the copper/bronze/Nb extrusion rod obtained in the step (3), removing a copper layer on the surface by adopting a peeling or grinding mode when the size is phi 15mm, and obtaining the bronze/Nb composite rod for preparing the Nb3Sn wire rod by the bronze method, wherein the processing rate of each drawing of the copper/bronze/Nb composite rod is 12%, the drawing speed is 5m/min, and the intermediate annealing is performed when the total processing rate of drawing is equal to 50%. The intermediate annealing temperature is 400 ℃, and the heat preservation time is 1 h.
Example four: the invention discloses a preparation method of copper-clad bronze/Nb composite rod
Step 1: cleaning porous bronze (Cu-15.5 wt.% Sn-0.3 wt.% Ti) ingots with an outer diameter of phi 110mm, a hole number of 19 holes, a hole diameter of phi 13.6mm, a spacing between holes of 4.1mm and a length of 350m, copper tubes with an outer diameter of phi 120mm and an inner diameter of phi 110mm, and 19 Nb rods with a diameter of phi 13.5 mm: firstly, removing oil stains on the surface by using a metal cleaner, and then cleaning a porous bronze ingot and a copper pipe by using a nitric acid solution with the volume concentration of 25%; and cleaning the Nb rod by using a mixed solution of 25% of nitric acid, 25% of hydrofluoric acid and the balance of water.
Step 2: loading a porous bronze ingot into a copper pipe, inserting Nb rods into holes in the porous bronze ingot, adding copper covers at two ends of the Nb rods for sealing and welding, wherein the vacuum degree in the welding process is less than 6.0 multiplied by 10 < -3 > Pa, and the welding current is 50mA, so as to obtain a copper/bronze/Nb sheath;
And step 3: the copper/bronze/Nb sheath is extruded after heat preservation for 2h at 600 ℃ to obtain a copper/bronze/Nb composite rod with the diameter of phi 40 mm;
And 4, step 4: and drawing the composite rod obtained by extrusion at a processing rate of 20%, wherein the drawing speed is 15m/min, and performing intermediate annealing after every three times of drawing. The intermediate annealing temperature is 520 ℃, and the heat preservation time is 1 h. And (3) processing the copper/bronze/Nb composite rod to phi 14.65mm, peeling to phi 13.2mm, and removing the copper layer coated on the surface to obtain the bronze/Nb composite rod for preparing the Nb3Sn wire rod by the bronze method.
the material does not crack in the processing process, and the bronze/Nb composite rod deforms uniformly.
Example five: the invention discloses a preparation method of copper-clad bronze/Nb composite rod
Step 1: cleaning a porous bronze (Cu-15.5 wt.% Sn-0.3 wt.% Ti) ingot with an outer diameter of phi 170mm, a number of holes of 37 holes, a diameter of phi 15.0mm, a spacing between holes of 3mm, a length of 550m, copper tubes with an outer diameter of phi 185mm and an inner diameter of phi 170mm, and 37 Nb rods with a diameter of phi 14.9 mm: firstly, removing oil stains on the surface by using a metal cleaner, and then cleaning a porous bronze ingot and a copper pipe by using a nitric acid solution with the volume concentration of 40%; and cleaning the Nb rod by using a mixed solution of 35% of nitric acid, 25% of hydrofluoric acid and the balance of water.
step 2: loading a porous bronze ingot into a copper pipe, inserting Nb rods into holes in the porous bronze ingot, adding copper covers at two ends of the Nb rods for sealing and welding, wherein the vacuum degree in the welding process is less than 6.0 multiplied by 10 < -3 > Pa, and the welding current is 60mA, so as to obtain a copper/bronze/Nb sheath;
And step 3: the copper/bronze/Nb sheath is extruded after heat preservation for 3h at 620 ℃ to obtain a copper/bronze/Nb composite rod with the diameter of phi 55 mm;
And 4, step 4: and drawing the composite rod obtained by extrusion at a processing rate of 20%, wherein the drawing speed is 15m/min, and performing intermediate annealing after every three times of drawing. The intermediate annealing temperature is 520 ℃, and the heat preservation time is 1 h. And (3) processing the copper/bronze/Nb composite rod to phi 14.4mm, peeling to phi 13mm, and removing the copper layer coated on the surface to obtain the bronze/Nb composite rod for preparing the bronze Nb3Sn wire rod.
The material does not crack in the processing process, and the bronze/Nb composite rod deforms uniformly.
example six: verification experiment of preparation method of copper-clad bronze/Nb composite rod
Compared with the bronze/Nb composite rods obtained by directly processing and annealing the bronze/Nb rods without being coated with copper, the bronze/Nb composite rods prepared by the first, fourth and fifth embodiments of the invention have no crack, the bronze/Nb composite rods prepared by the second and third embodiments of the invention have about 0.5% of crack, wherein the crack means that any crack of the prepared composite rods is the crack, and the crack rate of the bronze/Nb composite rods obtained by directly processing and annealing the bronze/Nb rods without being coated with copper exceeds 20%. Therefore, the method can effectively avoid the cracking of the bronze/Nb rod and obtain the uniform bronze/Nb composite rod.
As described above, the present invention can be preferably implemented, and the above-mentioned embodiments only describe the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the design spirit of the present invention should fall within the protection scope determined by the present invention.
Claims (10)
1. The preparation method of the bronze/Nb composite rod processed by copper-clad is characterized by comprising the following steps:
(1) Cleaning a copper pipe, a porous bronze ingot, and a Nb or Nb alloy rod;
(2) Putting a porous bronze ingot into a copper pipe, inserting a Nb or Nb alloy rod into the porous bronze ingot, adding copper covers at two ends of the porous bronze ingot, and sealing and welding by adopting an electron beam to obtain a copper/bronze/Nb composite sheath;
(3) Heating the multi-core bronze/Nb sheath obtained in the step (2) and then extruding to obtain a copper/bronze/Nb extrusion rod;
(4) And (4) repeatedly drawing and annealing the copper/bronze/Nb extrusion rod obtained in the step (3), and removing a copper layer on the surface in a scalping or grinding mode when the size is small to obtain the bronze/Nb composite rod for preparing the Nb3Sn wire rod by the bronze method.
2. The method for preparing a copper-clad bronze/Nb composite rod according to claim 1, wherein the mass percent of Sn in the porous bronze ingot in the step (1) is 13.5-16.0%, and the mass percent of Ti element is 0.2-0.4%.
3. the method for preparing a bronze/Nb composite rod processed by copper-clad according to claim 1, wherein the outer diameter of the porous bronze ingot in the step (1) is phi 110mm to phi 170mm, the number of the holes is 19 or 37, the diameter of the holes is phi 9mm to phi 23mm, the ratio of the distance between the holes to the diameter of the holes is 0.15-0.40, and the length is 300 mm-600 m; the outer diameter of the copper pipe is phi 120 mm-phi 185mm, the inner diameter of the copper pipe is consistent with the outer diameter of the porous bronze ingot, and the length of the copper pipe is 300 mm-600 m.
4. The method for manufacturing a copper-clad bronze/Nb composite rod according to claim 1, wherein the Nb alloy in the step (1) is an Nb-Ti rod with Ti content of 0.5-2.0% by mass, or an Nb-Ta rod with Ta content of 0.5-2.0% by mass.
5. The method for preparing a bronze/Nb composite rod processed by copper-clad according to claim 1, wherein the ratio of the sectional area of bronze to Nb or Nb alloy rod in the step (1) is 2.0 to 3.0.
6. the method for preparing a bronze/Nb composite rod processed by copper cladding according to claim 1, wherein the specific method for cleaning in the step (1) comprises the following steps: firstly, removing oil stains on the surface by using a metal cleaner, and then cleaning the bronze material by using a nitric acid solution, wherein the volume concentration of the nitric acid solution is 25-40%; the Nb or Nb alloy rod is cleaned by adopting a mixed solution of nitric acid, hydrofluoric acid and water, and the volume concentration of each component in the mixed solution is as follows: 25-35% of nitric acid, 15-25% of hydrofluoric acid and the balance of water.
7. The method for preparing a bronze/Nb composite rod processed by copper-clad according to claim 1, wherein in the step (2), the current of electron beam sealing welding is 30-100 mA, and the vacuum degree is less than 1.0 x 10 < -2 > Pa; in the step (3), the preheating temperature of the sheath is 550-670 ℃, the heat preservation time is 2-4 h, and the extrusion ratio is 8-15.
8. The method for manufacturing a copper-clad bronze/Nb composite rod according to claim 1, wherein the copper/bronze/Nb composite rod of step (4) is subjected to intermediate annealing when the copper/bronze/Nb composite rod is subjected to drawing at a rate of 12% to 25% per time, at a drawing speed of 5m/min to 20m/min, and at a total drawing rate of 50% or less.
9. The method for preparing a bronze/Nb composite rod processed by copper-clad according to claim 8, wherein the intermediate annealing temperature in the step (4) is 400-620 ℃, and the heat preservation time is 1-3 h.
10. The method for preparing a copper-clad bronze/Nb composite rod according to claim 9, wherein the copper layer coated on the surface of the copper/bronze/Nb composite rod in the step (4) is removed by peeling or grinding after the copper/bronze/Nb composite rod is processed to phi 15 mm.
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| CN201810595510.6A CN110580984B (en) | 2018-06-11 | 2018-06-11 | Preparation method of copper-clad bronze/Nb composite rod |
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