CN107578859A - A kind of preparation method of graphene/copper niobium Multicore composite material - Google Patents
A kind of preparation method of graphene/copper niobium Multicore composite material Download PDFInfo
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- CN107578859A CN107578859A CN201710792471.4A CN201710792471A CN107578859A CN 107578859 A CN107578859 A CN 107578859A CN 201710792471 A CN201710792471 A CN 201710792471A CN 107578859 A CN107578859 A CN 107578859A
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Abstract
The invention provides a kind of preparation method of graphene/copper niobium Multicore composite material, this method includes：First, copper scale and niobium powder high-energy ball milling are obtained refining powder；2nd, refinement powder is fitted into oxygen-free copper pipe and obtains tubulature complex；3rd, will be heat-treated after tubulature complex drawing；4th, the tubulature complex drawing after heat treatment is obtained into monofilamentary composite wire material；5th, 7 core composite wires are made in the once-combined shaping of monofilamentary composite wire material；6th, the 7 secondary composite moldings of core composite wire are made 72Core composite wire；7th, by 72Composite molding is made 7 to core composite wire three times3Core composite wire；8th, by 73Core composite wire loads the niobium pipe coated with graphene, and graphene/copper niobium composite wire is made in thermally treated and drawing；9th, graphene/copper niobium Multicore composite material is made through tubulature, soldering and sealing, hot extrusion and drawing in graphene/copper niobium composite wire, and the graphene uniform in the present invention is distributed in Multicore composite material, improves the intensity and electric conductivity of wire rod.
Description
Technical field
The invention belongs to high temperature superconductor technology field, and in particular to a kind of preparation of graphene/copper niobium Multicore composite material
Method.
Background technology
Copper alloy with high strength and high conductivity has because of the intensity with superelevation and excellent conductance in pulse magnetic field conductor field
And be widely applied.The copper alloy with high strength and high conductivity developed both at home and abroad at present mainly has：Cu/Nb-Ag、Cu/Nb-Cu、Cu-
Ag, Cu-Nb and Cu-Ta, wherein Cu-Nb alloys are because tensile strength and conductance matching are preferable, and preparation technology is simple, and cost is relatively low
As the first choice of pulse magnetic field material.
Graphene be by carbon atom form only one layer of atomic thickness two dimensional crystal, be have now been found that it is most thin, strong
A kind of novel nano-material that degree is maximum, electrical and thermal conductivity performance is most strong, 200 times more taller than best steel of its fracture strength.
Graphene also has stronger elastic performance, and stretch range can reach the 20% of own dimensions；Its resistivity ratio copper or silver are lower,
With excellent electric conductivity.
At present, Cu/Nb composites are mainly used in the conductor material of pulse magnet, are expected to be applied to high current transmission in the future
Wire and ELECTROMAGNETIC WEAPON, this performance to Cu/Nb composites propose very high requirement.Traditional Cu/Nb composite wire knots
Structure is using copper as matrix, and Nb core filaments are reinforcement, using bundle drawing method technology, by repeatedly compound and heat treatment technics prepare and
Into.The Cu/Nb wire rods prepared using this method can not be compound again, and already close to the theoretic limit, intensity is typically maintained in
Between 800MPa~900MPa, and the breakthrough of pulse magnet and ELECTROMAGNETIC WEAPON needs the intensity of wire rod in more than 1GPa, even more
It is high.At present, by graphene is doped to copper-based composite wire, promoting core size, further refinement and Cu/Nb interfaces are increased to carry
Rising the compound wire rod performances of Cu/Nb turns into study hotspot.Application publication number is to be disclosed in CN106448799A patent of invention
A kind of preparation method of graphene enhancing copper niobium Multicore composite material, first by Graphene powder, niobium powder and copper powder mixed processing, is obtained
The niobium copper composite powder of graphene enhancing, then obtains that intensity is larger, ductility is good and conductive by tubulature, drawing and composite molding
The strong copper niobium Multicore composite material of property；Graphene powder is prepared wire rod by the invention, and graphene divides in wire rod
Cloth is not uniform enough, easy conglomeration, is not easy to form layer structure, have impact on the intensity and electric conductivity of copper niobium Multicore composite material
Further improve.
The content of the invention
The technical problems to be solved by the invention are to be directed to above-mentioned the deficiencies in the prior art, there is provided a kind of graphene/copper
The preparation method of niobium Multicore composite material.Graphene fused solution is coated in niobium pipe outer wall by this method, is formed after solidification uniformly steady
Fixed graphene dispersion layer, graphene/copper niobium composite wire is prepared in conjunction with techniques such as heat treatment, drawing and hot extrusions, this is multiple
Zygonema material has the characteristics of intensity height and strong electric conductivity, and this method is flexible, suitable for preparing various shapes and chi
Very little Multicore composite material.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of graphene/copper niobium Multicore composite material
Preparation method, it is characterised in that this method comprises the following steps：
Step 1: carrying out high-energy ball milling after copper scale and niobium powder are well mixed, obtain refining powder；Copper scale and the niobium powder
Mass ratio be 1:1；The purity of the niobium powder is 99.99%；
Step 2: the refinement powder obtained in step 1 is fitted into the first oxygen-free copper pipe, then by the first oxygen-free copper pipe
Both ends sealed, obtain tubulature complex；It is described refinement powder charge weight for tubulature composite quality 10%~
60%；
Step 3: the tubulature complex obtained in step 2 is carried out into the drawing of multi-pass first, then it is heat-treated；Institute
The pass reduction for stating the first drawing is less than 10%；
Step 4: the tubulature complex after being heat-treated in step 3 is carried out into the drawing of multi-pass second, it is compound to obtain single
Wire rod；The pass reduction of second drawing is less than 15%；
Step 5: the monofilamentary composite wire material obtained in step 4 is carried out into once-combined shaping, 7 core composite wires are made；
The once-combined shaping uses clustered drawing, and the detailed process of the clustered drawing is：
Step 501, monofilamentary composite wire material is subjected to scale, shearing, aligning and pickling processes successively；
Step 502, the monofilamentary composite wire material boundling in 7 steps 501 after pickling processes is assembled into the second oxygen-free copper
Guan Zhong, then it is heat-treated, obtains copper pipe complex；
Step 503, by the copper pipe complex obtained in step 502 carry out the drawing of multi-pass the 3rd, obtain 7 core recombination lines
Material；The pass reduction of 3rd drawing is less than 21%；
Step 6: the 7 core composite wires obtained in step 5 are carried out into secondary composite molding, 7 are made2Core composite wire；
The method that the secondary composite molding uses is identical with the clustered drawing described in step 5；
Step 7: will be obtained in step 672Core composite wire carries out composite molding three times, is made 73Core composite wire；
The method that the composite molding three times uses is identical with the clustered drawing described in step 5；
Step 8: will be obtained in step 773Graphene/copper niobium composite wire, detailed process is made in core composite wire
For：
Step 801, graphene fused solution is coated uniformly on the outer wall of niobium pipe, graphene-niobium pipe is obtained after solidification；Institute
The graphene thickness stated in graphene-niobium pipe outer wall is less than 1mm；
Step 802, by 73Core composite wire is encased in graphene-niobium pipe, obtains composite pipe body；
Step 803, the composite pipe body obtained in step 802 is fitted into the 3rd oxygen-free copper pipe, carry out successively heat treatment and
The drawing of multi-pass the 4th, obtain graphene/copper niobium composite wire；The pass reduction of 4th drawing is less than 15%；
Step 9: graphene/copper niobium Multicore composite is made in the graphene obtained in step 8/copper niobium composite wire
Material, detailed process are：
Step 901, graphene/copper niobium composite wire blocked successively, is aligned, pickling and drying process；
Step 902, graphene/copper niobium composite wire in 19 steps 901 after drying process is taken to load the 4th oxygen-free copper
Guan Zhong, then fill the space in the 4th oxygen-free copper pipe between graphene/copper niobium composite wire with copper plunger, then to filling after
The both ends of 4th oxygen-free copper pipe carry out vacuum electron beam soldering and sealing；
Step 903, the 4th oxygen-free copper pipe after vacuum electron beam soldering and sealing is carried out to hot extrusion and the drawing of multi-pass the 5th successively
Pull out, obtain graphene/copper niobium Multicore composite material；The pass reduction of 5th drawing is less than 12%.
The preparation method of above-mentioned a kind of graphene/copper niobium Multicore composite material, it is characterised in that high described in step 1
The time of energy ball milling is 20h~40h.
The preparation method of above-mentioned a kind of graphene/copper niobium Multicore composite material, it is characterised in that Step 3: step 502
It it is 800 DEG C~1000 DEG C with the temperature being heat-treated described in step 803, the time is 60h.
The preparation method of above-mentioned a kind of graphene/copper niobium Multicore composite material, it is characterised in that single described in step 4
7 core composite wires described in core composite wire, step 5,7 described in step 627 described in core composite wire, step 73Core is answered
The shape of cross section of graphene described in zygonema material and step 8/copper niobium composite wire is regular hexagon；The regular hexagon
Opposite side distance be 2.5mm~2.7mm.
The preparation method of above-mentioned a kind of graphene/copper niobium Multicore composite material, it is characterised in that described in step 903
The temperature of hot extrusion is 600 DEG C~700 DEG C, and soaking time is 2h~6h, and extrusion ratio is 10~42.
The preparation process of graphene fused solution in step 801 is：First using crystalline flake graphite as raw material, using Hummers
Method prepares graphene oxide, and then using high-temperature reducing process, graphene oxide is placed in in closed reducing atmosphere the system that heats
Standby graphene, then melted under conditions of graphene is placed in into 900 DEG C~1000 DEG C and obtain graphene fused solution.
The present invention has advantages below compared with prior art：
1st, graphene fused solution is coated in niobium pipe outer wall by the present invention, increases the surface area of graphene, due to graphene
Layer structure with flowing, slip property is preferable, and niobium pipe can be dispersed in follow-up drawing and hot extrusion process
Outer wall, form stable graphene layer, be advantageous to give play to the features such as graphene intensity is high, ductility is good, electric conductivity is strong.
2nd, the graphene in the present invention and copper niobium composite wire prepare graphene/copper by heat treatment, drawing and hot extrusion
Niobium composite wire, the composite wire have the multilayer sandwiched structure of copper niobium composite wire-niobium pipe-graphene-copper pipe so that copper niobium
Between contact area increase, therefore the intensity of composite wire and electric conductivity improve.
3rd, the present invention carries out ball milling using high-energy ball milling to niobium powder and copper scale mixed-powder, makes the granularity of powder further thin
Change, powder mixing is more uniform, and the metallurgical binding between powder faster, refines powder after heat treatment, the expansion between copper niobium
Scattered degree is bigger, and the binding ability at copper niobium interface is improved.
4th, the copper-clad set of different size is encased in after the graphene in the present invention/copper niobium composite wire processing with copper plunger
In, graphene/copper niobium Multicore composite materials of a variety of shapes and sizes can be prepared through vacuum electron beam soldering and sealing, hot extrusion, drawing,
Flexible design, it is easy to adjust.
The present invention is described in further detail below by embodiment.
Embodiment
Embodiment 1
The present embodiment comprises the following steps：
Step 1: by the well mixed rear high-energy ball milling 20h of copper scale and niobium powder, obtain refining powder；Copper scale and the niobium powder
Mass ratio be 1:1；The purity of the niobium powder is 99.99%；
Step 2: by the refinement powder obtained in step 1 loading external diameter be 10.5mm, wall thickness 2.0mm, length be
In 400mm the first oxygen-free copper pipe, then the both ends of the first oxygen-free copper pipe are sealed, obtain tubulature complex；It is described thin
The charge weight for changing powder is the 10% of tubulature composite quality；
Step 3: the tubulature complex obtained in step 2 is carried out into the drawing of multi-pass first, the drawing die used is successively
For：Φ 10.3mm, Φ 9.89mm, Φ 9.43mm, Φ 9.2mm, Φ 8.86mm and Φ 8.66mm, wherein Φ represent circular drawing die
Diameter, then it is heat-treated 60h at 800 DEG C；The pass reduction of the drawing of multi-pass first is 4%~9%；
Step 4: the tubulature complex after being heat-treated in step 3 is subjected to the drawing of multi-pass second, the drawing die used
It is followed successively by：Φ8.5mm、Φ8.16mm、Φ7.97mm、Φ7.66mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ
6.0mm, Φ 5.57mm, Φ 5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：450℃/2h)、Φ
4.9mm、Φ4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ
3.26mm, Φ 3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm and S2.70mm, the circular drawing mode diameter of wherein Φ expressions, S
Six side's mould opposite side distances are represented, finally give the monofilamentary composite wire material that cross section is regular hexagon, the opposite side distance of the orthohexagonal is
2.70mm；
Step 5: the monofilamentary composite wire material obtained in step 4 is carried out into once-combined shaping, 7 core composite wires are made；
The once-combined shaping uses clustered drawing, and the detailed process of the clustered drawing is：
Step 501, monofilamentary composite wire material is subjected to scale, shearing, aligning and pickling processes successively；
Step 502, the monofilamentary composite wire material boundling in 7 steps 501 after pickling processes is assembled into external diameter it is
In 11.5mm, wall thickness 2.0mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 800 DEG C, is obtained
Copper pipe complex；
Step 503, by the copper pipe complex obtained in step 502 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ11.4mm、Φ10.87mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ8.16mm、Φ7.97mm、Φ7.74mm、
Φ 7.15mm, Φ 7.0mm, Φ 6.6mm, Φ 6.3mm, Φ 6.0mm, Φ 5.57mm, Φ 5.4mm, Φ 5.1mm, Φ 4.9mm (
Once made annealing treatment after this passage drawing：450℃/2h)、Φ4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ
4.0mm, Φ 3.81mm, Φ 3.68mm, Φ 3.4mm, Φ 3.26mm, Φ 3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm and
S2.70mm, wherein Φ represent circular drawing mode diameter, and S represents six side's mould opposite side distances, finally give cross section as regular hexagon
7 core composite wires, the opposite side distance of the regular hexagon is 2.70mm；
Step 6: the 7 core composite wires obtained in step 5 are carried out into secondary composite molding, 7 are made2Core composite wire；
The method that the secondary composite molding uses is identical with the clustered drawing described in step 5, the clustered drawing it is specific
Process is：
Step 601,7 core composite wires are subjected to scale, shearing, aligning and pickling processes successively；
Step 602,7 core composite wire boundlings in 7 steps 601 after pickling processes are assembled into external diameter it are
In 12.5mm, wall thickness 2.5mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 800 DEG C, is obtained
Copper pipe complex；
Step 603, by the copper pipe complex obtained in step 602 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ12.16mm、Φ11.97mm、Φ11.64mm、Φ11.4mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ
8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ5.57mm、Φ
5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：450℃/2h)、Φ4.9mm、Φ4.7mm、Φ
4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ
3.0mm, Φ 2.80mm, Φ 2.76mm and S2.70mm, the circular drawing mode diameter of wherein Φ expressions, S represent six side's mould opposite side distances,
Finally give 7 that cross section is regular hexagon2Core composite wire, the opposite side distance of the regular hexagon is 2.70mm；
Step 7: will be obtained in step 672Core composite wire carries out composite molding three times, is made 73Core composite wire；
The method that the composite molding three times uses is identical with the clustered drawing described in step 5, the clustered drawing it is specific
Process is：
Step 701, by 72Core composite wire carries out scale, shearing, aligning and pickling processes successively；
Step 702, by 7 steps 701 after pickling processes 72Core composite wire boundling is assembled into external diameter and is
In 12.5mm, wall thickness 2.5mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 800 DEG C, is obtained
Copper pipe complex；
Step 703, by the copper pipe complex obtained in step 702 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ12.16mm、Φ11.97mm、Φ11.64mm、Φ11.4mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ
8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ5.57mm、Φ
5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：450℃/2h)、Φ4.9mm、Φ4.7mm、Φ
4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ
3.0mm, Φ 2.80mm, Φ 2.76mm and S2.70mm, the circular drawing mode diameter of wherein Φ expressions, S represent six side's mould opposite side distances,
Finally give 7 that cross section is regular hexagon3Core composite wire, the opposite side distance of the regular hexagon is 2.70mm；
Step 8: will be obtained in step 773Graphene/copper niobium composite wire, detailed process is made in core composite wire
For：
Step 801, graphene fused solution is coated uniformly on to the outer wall that external diameter is 11.5mm, wall thickness is 1.67mm niobium pipes
On, graphene-niobium pipe is obtained after solidification；Graphene thickness in the graphene-niobium pipe outer wall is 0.1mm；
Step 802, by 73Core composite wire is encased in graphene-niobium pipe, obtains composite pipe body；
Step 803, by the composite pipe body obtained in step 802 loading external diameter be 13.5mm, wall thickness 1.0mm, length be
In 400mm the 3rd oxygen-free copper pipe, 60h is handled at 800 DEG C, then carries out the drawing of multi-pass the 4th, the drawing die used is successively
For：Φ8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ
5.57mm, Φ 5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：450℃/2h)、Φ4.9mm、Φ
4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ
3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm and S2.70mm, wherein Φ represent circular drawing mode diameter, and S represents six sides
Mould opposite side distance, finally gives graphene/copper niobium core composite wire that cross section is regular hexagon, and the opposite side distance of the regular hexagon is
2.70mm；
Step 9: graphene/copper niobium Multicore composite is made in the graphene obtained in step 8/copper niobium composite wire
Material, detailed process are：
Step 901, graphene/copper niobium composite wire blocked successively, is aligned, pickling and drying process；
Step 902, take graphene in 19 steps 901 after drying process/copper niobium composite wire to load external diameter to be
In 65.0mm, wall thickness 17.8mm, the 4th oxygen-free copper pipe that length is 200mm, then the 4th oxygen-free copper pipe is filled with copper plunger
Space between middle graphene/copper niobium composite wire, then vacuum electron beam is carried out to the both ends of the 4th oxygen-free copper pipe after filling
Soldering and sealing；
Step 903, by the 4th oxygen-free copper pipe after vacuum electron beam soldering and sealing in 600 DEG C of hot extrusion 2h, extrusion ratio 10, so
The drawing of multi-pass the 5th is carried out afterwards, and the drawing die used is followed successively by：Φ8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、
Φ 7.0mm, Φ 6.6mm and Φ 6.3mm, wherein Φ represent circular drawing mode diameter, obtain graphene/copper niobium Multicore composite
Material.
The core number of graphene manufactured in the present embodiment/copper niobium Multicore composite material is 19 × 73Core, after testing, the wire rod
Intensity is 664MPa, and the intensity of the same size wire rod prepared compared to conventional method improves 20%；The wire rod conductance is 67%
IACS, the resistivity of the same size wire rod prepared compared to conventional method reduce 9%.
Embodiment 2
The present embodiment comprises the following steps：
Step 1: by the well mixed rear high-energy ball milling 25h of copper scale and niobium powder, obtain refining powder；Copper scale and the niobium powder
Mass ratio be 1:1；The purity of the niobium powder is 99.99%；
Step 2: by the refinement powder obtained in step 1 loading external diameter be 10.5mm, wall thickness 2.0mm, length be
In 400mm the first oxygen-free copper pipe, then the both ends of the first oxygen-free copper pipe are sealed, obtain tubulature complex；It is described thin
The charge weight for changing powder is the 20% of tubulature composite quality；
Step 3: the tubulature complex obtained in step 2 is carried out into the drawing of multi-pass first, the drawing die used is successively
For：Φ 10.3mm, Φ 9.89mm, Φ 9.43mm, Φ 9.2mm, Φ 8.86mm and Φ 8.66mm, wherein Φ represent circular drawing die
Diameter, then it is heat-treated 60h at 850 DEG C；
Step 4: the tubulature complex after being heat-treated in step 3 is subjected to the drawing of multi-pass second, the drawing die used
It is followed successively by：Φ8.5mm、Φ8.16mm、Φ7.97mm、Φ7.66mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ
6.0mm, Φ 5.57mm, Φ 5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：500℃/2.5h)、Φ
4.9mm、Φ4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ
3.26mm, Φ 3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm and S2.60mm, the circular drawing mode diameter of wherein Φ expressions, S
Six side's mould opposite side distances are represented, finally give the monofilamentary composite wire material that cross section is regular hexagon, the opposite side distance of the orthohexagonal is
2.60mm；
Step 5: carrying out once-combined shaping to the monofilamentary composite wire material obtained in step 4,7 core composite wires are made；
The once-combined shaping uses clustered drawing, and the detailed process of the clustered drawing is：
Step 501, monofilamentary composite wire material is subjected to scale, shearing, aligning and pickling processes successively；
Step 502, the monofilamentary composite wire material boundling in 7 steps 501 after pickling processes is assembled into external diameter it is
In 11.5mm, wall thickness 2.0mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 850 DEG C, is obtained
Copper pipe complex；
Step 503, by the copper pipe complex obtained in step 502 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ11.4mm、Φ10.87mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ8.16mm、Φ7.97mm、Φ7.74mm、
Φ 7.15mm, Φ 7.0mm, Φ 6.6mm, Φ 6.3mm, Φ 6.0mm, Φ 5.57mm, Φ 5.4mm, Φ 5.1mm, Φ 4.9mm (
Once made annealing treatment after this passage drawing：500℃/2.5h)、Φ4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ
4.0mm, Φ 3.81mm, Φ 3.68mm, Φ 3.4mm, Φ 3.26mm, Φ 3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm and
S2.60mm, wherein Φ represent circular drawing mode diameter, and S represents six side's mould opposite side distances, finally give cross section as regular hexagon
7 core composite wires, the opposite side distance of the regular hexagon is 2.60mm；
Step 6: the 7 core composite wires obtained in step 5 are carried out into secondary composite molding, 7 are made2Core composite wire；
The method that the secondary composite molding uses is identical with the clustered drawing described in step 5, the clustered drawing it is specific
Process is：
Step 601,7 core composite wires are subjected to scale, shearing, aligning and pickling processes successively；
Step 602,7 core composite wire boundlings in 7 steps 601 after pickling processes are assembled into external diameter it are
In 12.5mm, wall thickness 2.5mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 850 DEG C, is obtained
Copper pipe complex；
Step 603, by the copper pipe complex obtained in step 602 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ12.16mm、Φ11.97mm、Φ11.64mm、Φ11.4mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ
8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ5.57mm、Φ
5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：500℃/2.5h)、Φ4.9mm、Φ4.7mm、Φ
4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ
3.0mm, Φ 2.80mm, Φ 2.76mm and S2.60mm, the circular drawing mode diameter of wherein Φ expressions, S represent six side's mould opposite side distances,
Finally give 7 that cross section is regular hexagon2Core composite wire, the opposite side distance of the regular hexagon is 2.60mm；
Step 7: will be obtained in step 672Core composite wire carries out composite molding three times, is made 73Core composite wire；
The method that the composite molding three times uses is identical with the clustered drawing described in step 5, the clustered drawing it is specific
Process is：
Step 701, by 72Core composite wire carries out scale, shearing, aligning and pickling processes successively；
Step 702, by 7 steps 701 after pickling processes 72Core composite wire boundling is assembled into external diameter and is
In 12.5mm, wall thickness 2.5mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 850 DEG C, is obtained
Copper pipe complex；
Step 703, by the copper pipe complex obtained in step 702 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ12.16mm、Φ11.97mm、Φ11.64mm、Φ11.4mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ
8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ5.57mm、Φ
5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：500℃/2.5h)、Φ4.9mm、Φ4.7mm、Φ
4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ
3.0mm, Φ 2.80mm, Φ 2.76mm, Φ 2.68mm and S2.60mm, wherein Φ represent circular drawing mode diameter, and S represents six sides
Mould opposite side distance, cross section is finally given as the 7 of regular hexagon3Core composite wire, the opposite side distance of the regular hexagon is 2.60mm；
Step 8: will be obtained in step 773Graphene/copper niobium composite wire, detailed process is made in core composite wire
For：
Step 801, graphene fused solution is coated uniformly on to the outer wall that external diameter is 11.5mm, wall thickness is 1.67mm niobium pipes
On, graphene-niobium pipe is obtained after solidification；Graphene thickness in the graphene-niobium pipe outer wall is 0.2mm；
Step 802, by 73Core composite wire is encased in graphene-niobium pipe, obtains composite pipe body；
Step 803, by the composite pipe body obtained in step 802 loading external diameter be 13.5mm, wall thickness 1.0mm, length be
In 400mm the 3rd oxygen-free copper pipe, 60h is handled at 850 DEG C, then carries out the drawing of multi-pass the 4th, the drawing die used is successively
For：Φ8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ
5.57mm, Φ 5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：500℃/2.5h)、Φ4.9mm、Φ
4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ
3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm and S2.60mm, wherein Φ represent circular drawing mode diameter, and S represents six sides
Mould opposite side distance, finally gives graphene/copper niobium core composite wire that cross section is regular hexagon, and the opposite side distance of the regular hexagon is
2.60mm；
Step 9: graphene/copper niobium Multicore composite is made in the graphene obtained in step 8/copper niobium composite wire
Material, detailed process are：
Step 901, graphene/copper niobium composite wire blocked successively, is aligned, pickling and drying process；
Step 902, take graphene in 19 steps 901 after drying process/copper niobium composite wire to load external diameter to be
In 65.0mm, wall thickness 17.8mm, the 4th oxygen-free copper pipe that length is 200mm, then the 4th oxygen-free copper pipe is filled with copper plunger
Space between middle graphene/copper niobium composite wire, then vacuum electron beam is carried out to the both ends of the 4th oxygen-free copper pipe after filling
Soldering and sealing；
Step 903, by the 4th oxygen-free copper pipe after vacuum electron beam soldering and sealing in 650 DEG C of hot extrusion 3h, extrusion ratio 20, so
The drawing of multi-pass the 5th is carried out afterwards, and the drawing die used is followed successively by：Φ8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、
Φ 7.0mm, Φ 6.6mm and Φ 6.3mm, wherein Φ represent circular drawing mode diameter, obtain graphene/copper niobium Multicore composite
Material.
The core number of graphene manufactured in the present embodiment/copper niobium Multicore composite material is 19 × 73Core, after testing, the wire rod
Intensity is 835MPa, and the intensity of the same size wire rod prepared compared to conventional method improves 25%；The wire rod conductance is 85%
IACS, the resistivity of the same size wire rod prepared compared to conventional method reduce 6%.
Embodiment 3
The present embodiment comprises the following steps：
Step 1: by the well mixed rear high-energy ball milling 30h of copper scale and niobium powder, obtain refining powder；Copper scale and the niobium powder
Mass ratio be 1:1；The purity of the niobium powder is 99.99%；
Step 2: by the refinement powder obtained in step 1 loading external diameter be 10.5mm, wall thickness 2.0mm, length be
In 400mm the first oxygen-free copper pipe, then the both ends of the first oxygen-free copper pipe are sealed, obtain tubulature complex；It is described thin
The charge weight for changing powder is the 30% of tubulature composite quality；
Step 3: the tubulature complex obtained in step 2 is carried out into the drawing of multi-pass first, the drawing die used is successively
For：Φ 10.3mm, Φ 9.89mm, Φ 9.43mm, Φ 9.2mm, Φ 8.86mm and Φ 8.66mm, wherein Φ represent circular drawing die
Diameter, then it is heat-treated 60h at 900 DEG C；
Step 4: the tubulature complex after being heat-treated in step 3 is subjected to the drawing of multi-pass second, the drawing die used
It is followed successively by：Φ8.5mm、Φ8.16mm、Φ7.97mm、Φ7.66mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ
6.0mm, Φ 5.57mm, Φ 5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：550℃/2.5h)、Φ
4.9mm、Φ4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ
3.26mm, Φ 3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm and S2.65mm, the circular drawing mode diameter of wherein Φ expressions, S
Six side's mould opposite side distances are represented, finally give the monofilamentary composite wire material that cross section is regular hexagon, the opposite side distance of the orthohexagonal is
2.65mm；
Step 5: the monofilamentary composite wire material obtained in step 4 is carried out into once-combined shaping, 7 core composite wires are made；
The once-combined shaping uses clustered drawing, and the detailed process of the clustered drawing is：
Step 501, monofilamentary composite wire material is subjected to scale, shearing, aligning and pickling processes successively；
Step 502, the monofilamentary composite wire material boundling in 7 steps 501 after pickling processes is assembled into external diameter it is
In 11.5mm, wall thickness 2.0mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 900 DEG C, is obtained
Copper pipe complex；
Step 503, step 503, by the copper pipe complex obtained in step 502 carry out the drawing of multi-pass the 3rd, use
Drawing die is followed successively by：Φ11.4mm、Φ10.87mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ8.16mm、Φ7.97mm、Φ
7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ5.57mm、Φ5.4mm、Φ5.1mm、Φ
4.9mm (is once made annealing treatment after this passage drawing：550℃/2.5h)、Φ4.7mm、Φ4.5mm、Φ4.3mm、Φ
4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ3.0mm、Φ2.80mm、
Φ 2.76mm and S2.65mm, the circular drawing mode diameter of wherein Φ expressions, S represent six side's mould opposite side distances, and finally giving cross section is
7 core composite wires of regular hexagon, the opposite side distance of the regular hexagon is 2.65mm；
Step 6: the 7 core composite wires obtained in step 5 are carried out into secondary composite molding, 7 are made2Core composite wire；
The method that the secondary composite molding uses is identical with the clustered drawing described in step 5, the clustered drawing it is specific
Process is：
Step 601,7 core composite wires are subjected to scale, shearing, aligning and pickling processes successively；
Step 602,7 core composite wire boundlings in 7 steps 601 after pickling processes are assembled into external diameter it are
In 12.5mm, wall thickness 2.5mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 900 DEG C, is obtained
Copper pipe complex；
Step 603, by the copper pipe complex obtained in step 602 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ12.16mm、Φ11.97mm、Φ11.64mm、Φ11.4mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ
8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ5.57mm、Φ
5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：550℃/2.5h)、Φ4.9mm、Φ4.7mm、Φ
4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ
3.0mm, Φ 2.80mm, Φ 2.76mm and S2.65mm, the circular drawing mode diameter of wherein Φ expressions, S represent six side's mould opposite side distances,
Finally give 7 that cross section is regular hexagon2Core composite wire, the opposite side distance of the regular hexagon is 2.65mm；
Step 7: will be obtained in step 672Core composite wire carries out composite molding three times, is made 73Core composite wire；
The method that the composite molding three times uses is identical with the clustered drawing described in step 5, the clustered drawing it is specific
Process is：
Step 701, by 72Core composite wire carries out scale, shearing, aligning and pickling processes successively；
Step 702, by 7 steps 701 after pickling processes 72Core composite wire boundling is assembled into external diameter and is
In 12.5mm, wall thickness 2.5mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 900 DEG C, is obtained
Copper pipe complex；
Step 703, by the copper pipe complex obtained in step 702 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ12.16mm、Φ11.97mm、Φ11.64mm、Φ11.4mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ
8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ5.57mm、Φ
5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：550℃/2.5h)、Φ4.9mm、Φ4.7mm、Φ
4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ
3.0mm, Φ 2.80mm, Φ 2.76mm, Φ 2.68mm and S2.65mm, wherein Φ represent circular drawing mode diameter, and S represents six sides
Mould opposite side distance, cross section is finally given as the 7 of regular hexagon3Core composite wire, the opposite side distance of the regular hexagon is 2.65mm；
Step 8: will be obtained in step 773Graphene/copper niobium composite wire, detailed process is made in core composite wire
For：
Step 801, graphene fused solution is coated uniformly on to the outer wall that external diameter is 11.5mm, wall thickness is 1.67mm niobium pipes
On, graphene-niobium pipe is obtained after solidification；Graphene thickness in the graphene-niobium pipe outer wall is 0.3mm；
Step 802, by 73Core composite wire is encased in graphene-niobium pipe, obtains composite pipe body；
Step 803, by the composite pipe body obtained in step 802 loading external diameter be 13.5mm, wall thickness 1.0mm, length be
In 400mm the 3rd oxygen-free copper pipe, 60h is handled at 900 DEG C, then carries out the drawing of multi-pass the 4th, the drawing die used is successively
For：Φ8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ
5.57mm, Φ 5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：550℃/2.5h)、Φ4.9mm、Φ
4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ
3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm and S2.65mm, wherein Φ represent circular drawing mode diameter, and S represents six sides
Mould opposite side distance, finally gives graphene/copper niobium core composite wire that cross section is regular hexagon, and the opposite side distance of the regular hexagon is
2.65mm；
Step 9: graphene/copper niobium Multicore composite is made in the graphene obtained in step 8/copper niobium composite wire
Material, detailed process are：
Step 901, graphene/copper niobium composite wire blocked successively, is aligned, pickling and drying process；
Step 902, take graphene in 19 steps 901 after drying process/copper niobium composite wire to load external diameter to be
In 65.0mm, wall thickness 17.8mm, the 4th oxygen-free copper pipe that length is 200mm, then the 4th oxygen-free copper pipe is filled with copper plunger
Space between middle graphene/copper niobium composite wire, then vacuum electron beam is carried out to the both ends of the 4th oxygen-free copper pipe after filling
Soldering and sealing；
Step 903, by the 4th oxygen-free copper pipe after vacuum electron beam soldering and sealing in 700 DEG C of hot extrusion 4h, extrusion ratio 30, so
The drawing of multi-pass the 5th is carried out afterwards, and the drawing die used is followed successively by：Φ8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、
Φ 7.0mm, Φ 6.6mm and Φ 6.3mm, wherein Φ represent circular drawing mode diameter, obtain graphene/copper niobium Multicore composite
Material.
The core number of graphene manufactured in the present embodiment/copper niobium Multicore composite material is 19 × 73Core, after testing, the wire rod
Intensity is 807MPa, and the intensity of the same size wire rod prepared compared to conventional method improves 18%；The wire rod conductance is 78%
IACS, the resistivity of the same size wire rod prepared compared to conventional method reduce 7%
Embodiment 4
The present embodiment comprises the following steps：
Step 1: by the well mixed rear high-energy ball milling 35h of copper scale and niobium powder, obtain refining powder；Copper scale and the niobium powder
Mass ratio be 1:1；The purity of the niobium powder is 99.99%；
Step 2: by the refinement powder obtained in step 1 loading external diameter be 10.5mm, wall thickness 2.0mm, length be
In 400mm the first oxygen-free copper pipe, then the both ends of the first oxygen-free copper pipe are sealed, obtain tubulature complex；It is described thin
The charge weight for changing powder is the 45% of tubulature composite quality；
Step 3: the tubulature complex obtained in step 2 is carried out into the drawing of multi-pass first, the drawing die used is successively
For：Φ 10.3mm, Φ 9.89mm, Φ 9.43mm, Φ 9.2mm, Φ 8.86mm and Φ 8.66mm, wherein Φ represent circular drawing die
Diameter, then it is heat-treated 60h at 950 DEG C；
Step 4: the tubulature complex after being heat-treated in step 3 is subjected to the drawing of multi-pass second, the drawing die used
It is followed successively by：Φ8.5mm、Φ8.16mm、Φ7.97mm、Φ7.66mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ
6.0mm, Φ 5.57mm, Φ 5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：450℃/2h)、Φ
4.9mm、Φ4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ
3.26mm, Φ 3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm, Φ 2.68mm and S2.55mm, wherein Φ represent circular and drawn
Withdrawing pattern diameter, S represent six side's mould opposite side distances, finally give the monofilamentary composite wire material that cross section is regular hexagon, the orthohexagonal
Opposite side distance be 2.55mm；
Step 5: the monofilamentary composite wire material obtained in step 4 is carried out into once-combined shaping, 7 core composite wires are made；
The once-combined shaping uses clustered drawing, and the detailed process of the clustered drawing is：
Step 501, monofilamentary composite wire material is subjected to scale, shearing, aligning and pickling processes successively；
Step 502, the monofilamentary composite wire material boundling in 7 steps 501 after pickling processes is assembled into external diameter it is
In 11.5mm, wall thickness 2.0mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 950 DEG C, is obtained
Copper pipe complex；
Step 503, by the copper pipe complex obtained in step 502 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ11.4mm、Φ10.87mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ8.16mm、Φ7.97mm、Φ7.74mm、
Φ 7.15mm, Φ 7.0mm, Φ 6.6mm, Φ 6.3mm, Φ 6.0mm, Φ 5.57mm, Φ 5.4mm, Φ 5.1mm, Φ 4.9mm (
Once made annealing treatment after this passage drawing：450℃/2h)、Φ4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ
4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ3.0mm、Φ2.80mm、Φ2.76mm、
Φ 2.68mm and S2.55mm, the circular drawing mode diameter of wherein Φ expressions, S represent six side's mould opposite side distances, and finally giving cross section is
7 core composite wires of regular hexagon, the opposite side distance of the regular hexagon is 2.55mm；
Step 6: the 7 core composite wires obtained in step 5 are carried out into secondary composite molding, 7 are made2Core composite wire；
The method that the secondary composite molding uses is identical with the clustered drawing described in step 5, the clustered drawing it is specific
Process is：
Step 601,7 core composite wires are subjected to scale, shearing, aligning and pickling processes successively；
Step 602,7 core composite wire boundlings in 7 steps 601 after pickling processes are assembled into external diameter it are
In 12.5mm, wall thickness 2.5mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 950 DEG C, is obtained
Copper pipe complex；
Step 603, by the copper pipe complex obtained in step 602 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ12.16mm、Φ11.97mm、Φ11.64mm、Φ11.4mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ
8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ5.57mm、Φ
5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：450℃/2h)、Φ4.9mm、Φ4.7mm、Φ
4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ
3.0mm, Φ 2.80mm, Φ 2.76mm, Φ 2.68mm and S2.55mm, wherein Φ represent circular drawing mode diameter, and S represents six sides
Mould opposite side distance, cross section is finally given as the 7 of regular hexagon2Core composite wire, the opposite side distance of the regular hexagon is 2.55mm；
Step 7: will be obtained in step 672Core composite wire carries out composite molding three times, is made 73Core composite wire；
The method that the composite molding three times uses is identical with the clustered drawing described in step 5, the clustered drawing it is specific
Process is：
Step 701, by 72Core composite wire carries out scale, shearing, aligning and pickling processes successively；
Step 702, by 7 steps 701 after pickling processes 72Core composite wire boundling is assembled into external diameter and is
In 12.5mm, wall thickness 2.5mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 950 DEG C, is obtained
Copper pipe complex；
Step 703, by the copper pipe complex obtained in step 702 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ12.16mm、Φ11.97mm、Φ11.64mm、Φ11.4mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ
8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ5.57mm、Φ
5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：450℃/2h)、Φ4.9mm、Φ4.7mm、Φ
4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ
3.0mm, Φ 2.80mm, Φ 2.76mm, Φ 2.68mm and S2.55mm, wherein Φ represent circular drawing mode diameter, and S represents six sides
Mould opposite side distance, cross section is finally given as the 7 of regular hexagon3Core composite wire, the opposite side distance of the regular hexagon is 2.55mm；
Step 8: will be obtained in step 773Graphene/copper niobium composite wire, detailed process is made in core composite wire
For：
Step 801, graphene fused solution is coated uniformly on to the outer wall that external diameter is 11.5mm, wall thickness is 1.67mm niobium pipes
On, graphene-niobium pipe is obtained after solidification；Graphene thickness in the graphene-niobium pipe outer wall is 0.4mm；
Step 802, by 73Core composite wire is encased in graphene-niobium pipe, obtains composite pipe body；
Step 803, by the composite pipe body obtained in step 802 loading external diameter be 13.5mm, wall thickness 1.0mm, length be
In 400mm the 3rd oxygen-free copper pipe, 60h is handled at 950 DEG C, then carries out the drawing of multi-pass the 4th, the drawing die used is successively
For：Φ8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ
5.57mm, Φ 5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：450℃/2h)、Φ4.9mm、Φ
4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ
3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm and S2.55mm, wherein Φ represent circular drawing mode diameter, and S represents six sides
Mould opposite side distance, finally gives graphene/copper niobium core composite wire that cross section is regular hexagon, and the opposite side distance of the regular hexagon is
2.55mm；
Step 9: graphene/copper niobium Multicore composite is made in the graphene obtained in step 8/copper niobium composite wire
Material, detailed process are：
Step 901, graphene/copper niobium composite wire blocked successively, is aligned, pickling and drying process；
Step 902, take graphene in 19 steps 901 after drying process/copper niobium composite wire to load external diameter to be
In 65.0mm, wall thickness 17.8mm, the 4th oxygen-free copper pipe that length is 200mm, then the 4th oxygen-free copper pipe is filled with copper plunger
Space between middle graphene/copper niobium composite wire, then vacuum electron beam is carried out to the both ends of the 4th oxygen-free copper pipe after filling
Soldering and sealing；
Step 903, by the 4th oxygen-free copper pipe after vacuum electron beam soldering and sealing in 700 DEG C of hot extrusion 5h, extrusion ratio 35, so
The drawing of multi-pass the 5th is carried out afterwards, and the drawing die used is followed successively by：Φ8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、
Φ 7.0mm, Φ 6.6mm and Φ 6.3mm, wherein Φ represent circular drawing mode diameter, obtain graphene/copper niobium Multicore composite
Material.
The core number of graphene manufactured in the present embodiment/copper niobium Multicore composite material is 19 × 73Core, after testing：The wire rod
Intensity is 536MPa, and the intensity of the same size wire rod prepared compared to conventional method improves 20%；The wire rod conductance is 77%
IACS, the resistivity of the same size wire rod prepared compared to conventional method reduce 9%.
Embodiment 5
The present embodiment comprises the following steps：
Step 1: by the well mixed rear high-energy ball milling 40h of copper scale and niobium powder, obtain refining powder；Copper scale and the niobium powder
Mass ratio be 1:1；The purity of the niobium powder is 99.99%；
Step 2: by the refinement powder obtained in step 1 loading external diameter be 10.5mm, wall thickness 2.0mm, length be
In 400mm the first oxygen-free copper pipe, then the both ends of the first oxygen-free copper pipe are sealed, obtain tubulature complex；It is described thin
The charge weight for changing powder is the 60% of tubulature composite quality；
Step 3: the tubulature complex obtained in step 2 is carried out into the drawing of multi-pass first, the drawing die used is successively
For：Φ 10.3mm, Φ 9.89mm, Φ 9.43mm, Φ 9.2mm, Φ 8.86mm and Φ 8.66mm, wherein Φ represent circular drawing die
Diameter, then it is heat-treated 60h at 1000 DEG C；
Step 4: the tubulature complex after being heat-treated in step 3 is subjected to the drawing of multi-pass second, the drawing die used
It is followed successively by：Φ8.5mm、Φ8.16mm、Φ7.97mm、Φ7.66mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ
6.0mm, Φ 5.57mm, Φ 5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：650℃/4h)、Φ
4.9mm、Φ4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ
3.26mm, Φ 3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm, Φ 2.68mm and S2.50mm, wherein Φ represent circular and drawn
Withdrawing pattern diameter, S represent six side's mould opposite side distances, finally give the monofilamentary composite wire material that cross section is regular hexagon, the orthohexagonal
Opposite side distance be 2.50mm；
Step 5: the monofilamentary composite wire material obtained in step 4 is carried out into once-combined shaping, 7 core composite wires are made；
The once-combined shaping uses clustered drawing, and the detailed process of the clustered drawing is：
Step 501, monofilamentary composite wire material is subjected to scale, shearing, aligning and pickling processes successively；
Step 502, the monofilamentary composite wire material boundling in 7 steps 501 after pickling processes is assembled into external diameter it is
In 11.5mm, wall thickness 2.0mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 1000 DEG C, is obtained
Copper pipe complex；
Step 503, by the copper pipe complex obtained in step 502 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ11.4mm、Φ10.87mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ8.16mm、Φ7.97mm、Φ7.74mm、
Φ 7.15mm, Φ 7.0mm, Φ 6.6mm, Φ 6.3mm, Φ 6.0mm, Φ 5.57mm, Φ 5.4mm, Φ 5.1mm, Φ 4.9mm (
Once made annealing treatment after this passage drawing：650℃/4h)、Φ4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ
4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ3.0mm、Φ2.80mm、Φ2.76mm、
Φ 2.68mm and S2.50mm, the circular drawing mode diameter of wherein Φ expressions, S represent six side's mould opposite side distances, and finally giving cross section is
7 core composite wires of regular hexagon, the opposite side distance of the regular hexagon is 2.50mm；
Step 6: the 7 core composite wires obtained in step 5 are carried out into secondary composite molding, 7 are made2Core composite wire；
The method that the secondary composite molding uses is identical with the clustered drawing described in step 5, the clustered drawing it is specific
Process is：
Step 601,7 core composite wires are subjected to scale, shearing, aligning and pickling processes successively；
Step 602,7 core composite wire boundlings in 7 steps 601 after pickling processes are assembled into external diameter it are
In 12.5mm, wall thickness 2.5mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 1000 DEG C, is obtained
Copper pipe complex；
Step 603, by the copper pipe complex obtained in step 602 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ12.16mm、Φ11.97mm、Φ11.64mm、Φ11.4mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ
8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ5.57mm、Φ
5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：650℃/4h)、Φ4.9mm、Φ4.7mm、Φ
4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ
3.0mm, Φ 2.80mm, Φ 2.76mm, Φ 2.68mm and S2.50mm, wherein Φ represent circular drawing mode diameter, and S represents six sides
Mould opposite side distance, cross section is finally given as the 7 of regular hexagon2Core composite wire, the opposite side distance of the regular hexagon is 2.50mm；
Step 7: will be obtained in step 672Core composite wire carries out composite molding three times, is made 73Core composite wire；
The method that the composite molding three times uses is identical with the clustered drawing described in step 5, the clustered drawing it is specific
Process is：
Step 701, by 72Core composite wire carries out scale, shearing, aligning and pickling processes successively；
Step 702, by 7 steps 701 after pickling processes 72Core composite wire boundling is assembled into external diameter and is
In 12.5mm, wall thickness 2.5mm, the second oxygen-free copper pipe that length is 400mm, then the isothermal holding 60h at 1000 DEG C, is obtained
Copper pipe complex；
Step 703, by the copper pipe complex obtained in step 702 carry out the drawing of multi-pass the 3rd, the drawing die used according to
It is secondary to be：Φ12.16mm、Φ11.97mm、Φ11.64mm、Φ11.4mm、Φ10.3mm、Φ9.2mm、Φ8.5mm、Φ
8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ5.57mm、Φ
5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：650℃/4h)、Φ4.9mm、Φ4.7mm、Φ
4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ3.13mm、Φ
3.0mm, Φ 2.80mm, Φ 2.76mm, Φ 2.68mm and S2.50mm, wherein Φ represent circular drawing mode diameter, and S represents six sides
Mould opposite side distance, cross section is finally given as the 7 of regular hexagon3Core composite wire, the opposite side distance of the regular hexagon is 2.50mm；
Step 8: will be obtained in step 773Graphene/copper niobium composite wire, detailed process is made in core composite wire
For：
Step 801, graphene fused solution is coated uniformly on to the outer wall that external diameter is 11.5mm, wall thickness is 1.67mm niobium pipes
On, graphene-niobium pipe is obtained after solidification；Graphene thickness in the graphene-niobium pipe outer wall is 0.5mm；
Step 802, by 73Core composite wire is encased in graphene-niobium pipe, obtains composite pipe body；
Step 803, by the composite pipe body obtained in step 802 loading external diameter be 13.5mm, wall thickness 1.0mm, length be
In 400mm the 3rd oxygen-free copper pipe, 60h is handled at 1000 DEG C, then carries out the drawing of multi-pass the 4th, the drawing die used is successively
For：Φ8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、Φ7.0mm、Φ6.6mm、Φ6.3mm、Φ6.0mm、Φ
5.57mm, Φ 5.4mm, Φ 5.1mm (are once made annealing treatment after this passage drawing：650℃/4h)、Φ4.9mm、Φ
4.7mm、Φ4.5mm、Φ4.3mm、Φ4.13mm、Φ4.0mm、Φ3.81mm、Φ3.68mm、Φ3.4mm、Φ3.26mm、Φ
3.13mm, Φ 3.0mm, Φ 2.80mm, Φ 2.76mm and S2.50mm, wherein Φ represent circular drawing mode diameter, and S represents six sides
Mould opposite side distance, finally gives graphene/copper niobium core composite wire that cross section is regular hexagon, and the opposite side distance of the regular hexagon is
2.50mm；
Step 9: graphene/copper niobium Multicore composite is made in the graphene obtained in step 8/copper niobium composite wire
Material, detailed process are：
Step 901, graphene/copper niobium composite wire blocked successively, is aligned, pickling and drying process；
Step 902, take graphene in 19 steps 901 after drying process/copper niobium composite wire to load external diameter to be
In 65.0mm, wall thickness 17.8mm, the 4th oxygen-free copper pipe that length is 200mm, then the 4th oxygen-free copper pipe is filled with copper plunger
Space between middle graphene/copper niobium composite wire, then vacuum electron beam is carried out to the both ends of the 4th oxygen-free copper pipe after filling
Soldering and sealing；
Step 903, by the 4th oxygen-free copper pipe after vacuum electron beam soldering and sealing in 700 DEG C of hot extrusion 6h, extrusion ratio 42, so
The drawing of multi-pass the 5th is carried out afterwards, and the drawing die used is followed successively by：Φ8.16mm、Φ7.97mm、Φ7.74mm、Φ7.15mm、
Φ 7.0mm, Φ 6.6mm and Φ 6.3mm, wherein Φ represent circular drawing mode diameter, obtain graphene/copper niobium Multicore composite
Material.
The core number of graphene manufactured in the present embodiment/copper niobium Multicore composite material is 19 × 73Core, after testing：The wire rod
Intensity is 724MPa, and the intensity of the same size wire rod prepared compared to conventional method improves 15%；The wire rod conductance is 81%
IACS, the resistivity of the same size wire rod prepared compared to conventional method reduce 8%.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions.It is every according to invention skill
Any simple modification, change and equivalence change that art is substantially made to above example, still fall within technical solution of the present invention
Protection domain in.
Claims (5)
1. the preparation method of a kind of graphene/copper niobium Multicore composite material, it is characterised in that this method comprises the following steps：
Step 1: carrying out high-energy ball milling after copper scale and niobium powder are well mixed, obtain refining powder；The matter of copper scale and the niobium powder
The ratio between amount is 1:1；The purity of the niobium powder is 99.99%；
Step 2: the refinement powder obtained in step 1 is fitted into the first oxygen-free copper pipe, then by the two of the first oxygen-free copper pipe
End is sealed, and obtains tubulature complex；The charge weight of the refinement powder is the 10%~60% of tubulature composite quality；
Step 3: the tubulature complex obtained in step 2 is carried out into the drawing of multi-pass first, then it is heat-treated；Described
The pass reduction of one drawing is less than 10%；
Step 4: the tubulature complex after being heat-treated in step 3 is carried out into the drawing of multi-pass second, monofilamentary composite wire material is obtained；
The pass reduction of second drawing is less than 15%；
Step 5: the monofilamentary composite wire material obtained in step 4 is carried out into once-combined shaping, 7 core composite wires are made；It is described
Once-combined shaping uses clustered drawing, and the detailed process of the clustered drawing is：
Step 501, monofilamentary composite wire material is subjected to scale, shearing, aligning and pickling processes successively；
Step 502, the monofilamentary composite wire material boundling in 7 steps 501 after pickling processes is assembled into the second oxygen-free copper pipe,
Then it is heat-treated, obtains copper pipe complex；
Step 503, by the copper pipe complex obtained in step 502 carry out the drawing of multi-pass the 3rd, obtain 7 core composite wires；Institute
The pass reduction for stating the 3rd drawing is less than 21%；
Step 6: the 7 core composite wires obtained in step 5 are carried out into secondary composite molding, 7 are made2Core composite wire；Described two
The method that secondary composite molding uses is identical with the clustered drawing described in step 5；
Step 7: will be obtained in step 672Core composite wire carries out composite molding three times, is made 73Core composite wire；It is described
The method that composite molding uses three times is identical with the clustered drawing described in step 5；
Step 8: will be obtained in step 773Graphene/copper niobium composite wire is made in core composite wire, and detailed process is：
Step 801, graphene fused solution is coated uniformly on the outer wall of niobium pipe, graphene-niobium pipe is obtained after solidification；The stone
Graphene thickness in black alkene-niobium pipe outer wall is less than 1mm；
Step 802, by 73Core composite wire is encased in graphene-niobium pipe, obtains composite pipe body；
Step 803, the composite pipe body obtained in step 802 is fitted into the 3rd oxygen-free copper pipe, is heat-treated successively and multiple tracks
Secondary 4th drawing, obtain graphene/copper niobium composite wire；The pass reduction of 4th drawing is less than 15%；
Step 9: the graphene obtained in step 8/copper niobium composite wire is made into graphene/copper niobium Multicore composite material, have
Body process is：
Step 901, graphene/copper niobium composite wire blocked successively, is aligned, pickling and drying process；
Step 902, graphene/copper niobium composite wire in 19 steps 901 after drying process is taken to be fitted into the 4th oxygen-free copper pipe,
Then the space in the 4th oxygen-free copper pipe between graphene/copper niobium composite wire is filled with copper plunger, then to the 4th after filling
The both ends of oxygen-free copper pipe carry out vacuum electron beam soldering and sealing；
Step 903, the 4th oxygen-free copper pipe after vacuum electron beam soldering and sealing is subjected to hot extrusion and the drawing of multi-pass the 5th successively, obtained
To graphene/copper niobium Multicore composite material；The pass reduction of 5th drawing is less than 12%.
A kind of 2. preparation method of graphene according to claim 1/copper niobium Multicore composite material, it is characterised in that step
The time of high-energy ball milling described in rapid one is 20h~40h.
A kind of 3. preparation method of graphene according to claim 1/copper niobium Multicore composite material, it is characterised in that step
The temperature being heat-treated described in rapid three, step 502 and step 803 is 800 DEG C~1000 DEG C, and the time is 60h.
A kind of 4. preparation method of graphene according to claim 1/copper niobium Multicore composite material, it is characterised in that step
Monofilamentary composite wire material described in rapid four, 7 core composite wires described in step 5,7 described in step 62Core composite wire, step
7 described in seven3The shape of cross section of graphene described in core composite wire and step 8/copper niobium composite wire is positive six side
Shape；The opposite side distance of the regular hexagon is 2.5mm~2.7mm.
A kind of 5. preparation method of graphene according to claim 1/copper niobium Multicore composite material, it is characterised in that step
The temperature of hot extrusion described in rapid 903 is 600 DEG C~700 DEG C, and soaking time is 2h~6h, and extrusion ratio is 10~42.
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