CN110465643A - A kind of preparation method of copper niobium composite material - Google Patents
A kind of preparation method of copper niobium composite material Download PDFInfo
- Publication number
- CN110465643A CN110465643A CN201910862326.8A CN201910862326A CN110465643A CN 110465643 A CN110465643 A CN 110465643A CN 201910862326 A CN201910862326 A CN 201910862326A CN 110465643 A CN110465643 A CN 110465643A
- Authority
- CN
- China
- Prior art keywords
- niobium
- copper
- composite material
- mold
- niobium composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D19/00—Casting in, on, or around objects which form part of the product
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
- C22F1/18—High-melting or refractory metals or alloys based thereon
Abstract
The invention discloses a kind of preparation method of copper niobium composite material, each component chemical quality percentage in the copper niobium composite material are as follows: content of niobium 10-20%, surplus are copper.Molten metal copper liquid is poured into the mold embedded with niobium stick by the present invention, and the solid-liquid to realize copper and niobium is compound, prepares copper niobium composite material blank.Using the plastic processings means such as multi-pass hot forging and cold rolling, while so that niobium phase size is refined to nanometer scale, high density dislocation is introduced, obtains copper niobium composite material high-intensitive.The tensile strength of material is 700-1050MPa, conductivity 65-85%IACS, can satisfy high-strength magnetic field field to the practical application request of high amplitude pulses magnetic field magnet material.
Description
Technical field
The invention belongs to non-ferrous metals processing fields, are related to a kind of preparation method of high-strength copper niobium composite material.
Background technique
In high-intensity magnetic field field, copper alloy with high strength and high conductivity is commonly used for pulsed magnetic field magnet material.On the one hand, the high intensity of material
It can be made to bear bigger Lorentz force in the operational process of magnetic field；On the other hand, the excellent electric conductivity of material is effectively reduced
The Joule heat generated in the operational process of magnetic field.For superelevation strong pulsed magnetic field (such as arteries and veins of 100 T for further developing higher intensity
Rush magnetic field), intensity and electric conductivity to magnet material propose requirements at the higher level.Copper niobium composite material is that one kind has both high-intensitive and height
The structure function material of electric conductivity is the superelevation strong pulsed magnetic field magnet material of great application potential.
After copper niobium composite material passes through severe plastic deformation, copper, niobium two-phase reach nanometer amount in one-dimensional or two-dimensional directional
Grade, to obtain high intensity.In addition, the mutual solubility of niobium and copper is minimum.In room temperature, solubility of the copper in niobium is lower than
0.1at.%, solubility of the niobium in copper are lower than 0.02at%.Electric conductivity shadow of the presence of niobium to Copper substrate in copper niobium composite material
Sound is small, i.e. material still has excellent electric conductivity after adding a large amount of niobium elements.
Currently, the preparation process of reported copper niobium composite material mainly include the following types:
First method is to realize that copper, the physics of niobium phase are compound by severe plastic deformations methods such as accumulation pack rolling, technology drawings.
In addition, the nanosizing of copper, niobium two-phase is realized during severe plastic deformation, to obtain the copper niobium of high-intensitive, high conductivity
Composite material.The major defect of this method is that process is many and diverse, and equipment requirement is high, and the production cycle is long, it is difficult to which preparation is big
The blocky copper niobium composite material of size.
Second method is the mechanical alloying method of copper powder and niobium powder to be realized by high-energy ball milling, then pass through powder metallurgy hand
Section prepares high-performance copper niobium composite material.The major defect of this method is to be difficult to prepare large product, and high production cost.
The third method is copper-niobium alloys ingot casting to be prepared by induction melting and consumable arc-melting technique, then use multiple tracks
The high-strength high-conductivity copper niobium composite material that niobium mutually reaches nanometer scale is made in the means such as secondary drawing or rolling.However, niobium fusing point it is high and
It is insoluble in metal copper liquid, by taking Cu-20Nb alloy as an example, is completely dissolved niobium element in the process, smelting temperature need to reach
2200 DEG C or more.Traditional copper alloy casting method is difficult to prepare copper-niobium alloys ingot casting, it is necessary to using induction melting with from power consumption
The method that arc melting combines prepares copper-niobium alloys blank.The major defect of this method be smelting technology complexity, alloy at
Stability is divided to be difficult to control, high production cost.
Therefore, how to simplify the preparation method of copper niobium composite material, realize large scale high-strength high-conductivity copper niobium composite material
Efficiently preparation, is letter technical problem to be solved.
Summary of the invention
For the deficiency of existing copper niobium composite material processing technology of preparing, present invention seek to address that existing copper niobium composite material
The problems such as founding and processing technology are complicated, finished size is limited.
In view of the above problems, it is an object of the present invention to propose a kind of copper niobium composite material system easy to operate and safe
Preparation Method.Molten metal copper liquid is poured into the mold embedded with niobium stick, realizes that copper, the solid-liquid of niobium are compound, it is multiple to prepare copper niobium
Condensation material；By the means such as multi-pass hot forging and cold rolling, niobium Xiang Yutong phase size can be not only refined, and can be introduced a large amount of
Dislocation, so that the copper niobium composite material with high strength & high electric-conduction is made, suitable for high amplitude pulses magnetic field magnet material.
To achieve the goals above, the present invention adopts the following technical scheme that realization:
A kind of preparation method of copper niobium composite material, which comprises the following steps:
Step 1: production mold, the mold is made of the first component and the docking of second component level, the side of mold inner-cavity by
Channel is poured up to being arranged with；The area for removing casting channel part is effective area, if uniformly distributed in the effective area
Dry niobium stick mounting hole, the niobium in niobium stick alloy are mounted in the niobium stick mounting hole in the form of niobium stick；
Step 2: niobium stick made of several pure niobiums is horizontally inserted into the niobium stick mounting hole, the first component with it is described
The height and width of second component composition mold inner-cavity are all larger than 5 times of thickness or more of mold；
Step 3: fine copper is packed into graphite crucible, and it is put into vacuum induction melting furnace, by the vacuum in vacuum induction melting furnace
Degree should be reduced to 6.0 × 10-2Pa or less；Be filled with protective gas, melt copper under protective atmosphere, smelting temperature at 1200 DEG C extremely
Between 1450 DEG C；Heat preservation 5 to 10 minutes injects mold inner-cavity from the casting channel of mold；Billet is formed after cooling；
Step 4: the billet is carried out crop end and milling face, surface oxide layer is eliminated, the extra fine copper in excision side obtains
The compound square billet of copper niobium；
0.5 to 1 hour is kept the temperature Step 5: the compound square billet of copper niobium is put into 700 DEG C to 800 DEG C of heating furnace；
Step 6: being hot-forged to the compound square billet of copper niobium, hot forging temperature is not less than 450 DEG C；After hot forging, with niobium mandrel to flat
The strain of line direction is greater than 1.5；
Step 7: the compound square billet of copper niobium is put into keep the temperature 0.5 to 1 hour in 800 DEG C to 900 DEG C of heating furnace after carry out heat
Forging；It is greater than 1.2 in the normal strain being parallel on the long direction of the shortest edge；
Step 8: step 7 at least repeats 28 times；
Step 9: the compound square billet of copper niobium is carried out milling face and pickling processes, after pickling, dehydration and drying；Cold rolling is carried out,
It rolls reduction ratio and is greater than 97.3%, obtain copper niobium composite board.
Further, the diameter of the niobium stick mounting hole is 0.5-4mm, and depth 5-10mm, two pitchs of holes are greater than 2mm.
Further, the width in the casting channel is greater than 40mm.
Further, the quality purity of the pure niobium and fine copper is not less than 99.9%.
Further, material temperature is greater than 450 DEG C in entire hot forging process in step 6 and step 7, when temperature is in 450-
500 DEG C, continue hot forging process after material is put into 700-800 DEG C of heat preservation 0.5h.
Further, between 10% to 20, surplus is copper and can not go the mass percent of niobium in the copper niobium composite material
The impurity removed.
η calculation formula is strained in the present invention as the expression of η=ln (L/L0) length available, wherein L0 and L is respectively that material exists
Length before and after deformation.
Two pitchs of holes are expressed as distance between the two hole centers of circle and subtract two pore radius in the present invention.For example, the two of hole A and hole B
Distance-hole A radius-hole B radius between pitch of holes=hole A and the hole center of circle B.
KAM (Kernel Average Misorientation) value of copper phase in material is measured in the present invention using EBSD,
The value reflects the average orientation difference and dislocation density of material domain.Material KAM value is associated with close with the dislocation density of material internal
It cuts, KAM value is bigger, and dislocation density is higher.
The invention has the following beneficial effects:
1) present invention in molten metal copper liquid is poured into the mold embedded with solid-state niobium stick, by solid-liquid composite algorithm realize copper with
The chemical bonding of niobium, to prepare copper niobium composite material billet.The preparation method of copper niobium composite material billet is simply easy in the present invention
Row.
2) it is hot-forged by multi-pass, folds, is broken, the niobium phase in refinement copper niobium composite material, and being uniformly distributed niobium mutually
In material.
3) pass through cold rolling, on the one hand, niobium phase size can be further decreased, it is made to reach a nanometer ruler in one-dimensional direction
Degree, thus the interface enhancing effect of reinforcing material；On the other hand, a large amount of dislocations, reinforcing material dislocation strengthening effect can be introduced.
Under the action of these two aspects factor, so that the intensity of copper niobium composite material further increases.
4) average-size of copper alloy of the present invention niobium phase thickness after completing hot forging is less than 4 μm；Niobium is mutually rolling face normal direction
Average thickness is less than 80nm；In addition, rolling the KAM value of the copper phase in face between 2.5-4.0 using EBSD method measurement material；With excellent
Good high strength & high electric-conduction, the copper niobium composite material tensile strength be 750-1050MPa, conductivity 65-85%IACS,
Excellent combination property, suitable for high amplitude pulses magnetic field magnet material.
The present invention provides a kind of simple and easy on the basis of copper niobium composite material itself has high strength & high electric-conduction
Preparation for processing, have apparent technical advantage.
Detailed description of the invention
Fig. 1 is preparation method flow chart of the invention；
Fig. 2 is the structural schematic diagram of inventive die after assembling.
In figure: 1, left mold；2, niobium stick；3, right mould has；4, niobium stick mounting hole.
Specific embodiment
In order to which the present invention is further explained, the preferred embodiment of the invention is described below with reference to embodiment.Implement
The description of example is not construed as any limitation of the invention only to further illustrate feature and advantage of the invention.
Embodiment 1
The preparation of Cu-10wt%Nb composite board:
As shown in Figure 1, content of niobium is the preparation of the copper niobium composite board of 10wt%, specifically implement according to the following steps:
Step 1: processing multiple groups circular hole on the 1 inner wall front of left mold of casting mould as niobium stick mounting hole 4, circular hole is in battle array
Column arrangement.Circularhole diameter is 2.7mm, and depth 6mm, two pitchs of holes are 4.3mm, the most narrow spacing of circular hole Kong Xinyu mold left side
From for 52mm, which should be not less than 40mm；To reserve casting channel on the left side；Channel can also will be poured to be arranged on right side.
Multiple groups circular hole can be also processed as niobium stick mounting hole 4 on the inner wall front that right mould has 3, only, both sides are respectively provided with mounting hole
It installs more troublesome.Left 1 inner wall front of mold removes the area that casting channel occupies, and residual area is effective area；Niobium stick peace
The setting for filling hole should be in effective area region.By the diameter and radical that calculate niobium stick mounting hole 4, it is ensured that effective area
In region, the ratio of niobium and copper meets design requirement.
Step 2: being 2.6mm by diameter, length is quality 10.35 niobium stick 2 totally 3249 made of the pure niobium of 70mm
Kilogram, it is embedded in the niobium stick mounting hole 4 of left mold 1, and right mould tool 3 combine completion with left mold 1.Mold cavity be it is rectangular,
Type chamber height, length and width are respectively 560mm, 460mm and 65mm.Niobium stick diameter should be 0.02mm- smaller than Die orifice diameter
0.2mm guarantees that niobium stick can be smoothly embedded in mold circular hole.
Step 3: fine copper is packed into graphite crucible, and it is put into vacuum induction melting furnace.It will be in vacuum induction melting furnace
Vacuum degree is reduced to 5.8 × 10-2Pa is subsequently passed protective gas such as argon gas.Vacuum degree in vacuum induction melting furnace should reduce
To 6.0 × 10-2Pa or less.Metallic copper is melted under an argon atmosphere, smelting temperature is 1400 DEG C；Smelting temperature should be at 1200 DEG C
To between 1450 DEG C.Cast gate is being kept the temperature close to mold left side, molten metal copper liquid at least after ten minutes, from mold left side
It injects in mold.After metal liquid is cooling, ingot casting and mold are taken out.After removing mold, it is rectangular to obtain copper niobium composite material
Billet.The quality purity of above-mentioned pure niobium and fine copper is not less than 99.9%.
Step 4: copper niobium composite material billet described in step 3 is carried out crop end and milling face, surface oxide layer is eliminated,
Cut off the extra fine copper in side, obtain height, length and width be respectively 400mm, 400mm and 60mm the compound square billet of copper niobium；
Wherein the content of niobium is 8.87 kilograms；The content of copper is 76.23 kilograms.
Step 5: copper niobium composite material billet described in step 4 is put into the heating furnace inside holding 1h that temperature is 900 DEG C.
Step 6: copper niobium composite material described in step 5 is hot-forged, material temperature in hot forging process be should be greater than
450 DEG C, when temperature reaches 450 DEG C, continue hot forging process after material is put into 900 DEG C of heat preservation 0.5h.Copper niobium composite wood after hot forging
The length of material foreshortens to about 80mm by 400mm, and height still keeps 400mm, and width rises to about 300mm by 60mm, and copper niobium is compound
Material reaches 1.6 in the strain with niobium mandrel to parallel direction.
Step 7: being hot-forged after copper niobium composite material described in step 6 is put into 750 DEG C of heat preservation 1h, material had been hot-forged
Temperature should be greater than 450 DEG C in journey, when temperature reaches 450 DEG C, continue hot forging process after material is put into 750 DEG C of heat preservation 0.5h.Copper
After the hot forging of niobium composite material, the shortest edge is the first rib；The long 300mm that rises to by 80mm of first rib, the longest edge are the second rib；
Second rib is long to foreshorten to 80mm by 400mm, and third rib is long to rise to 400mm by 300mm, and material is to be parallel to the shortest edge long ---
Normal strain on the long direction of first rib is up to 1.32(ln (300/80)).After hot forging, the first rib becomes new third rib；
Second rib becomes the first new rib；Third rib becomes the second new rib.
Step 8: repeating operation 28 times of step 7, refinement copper phase and niobium phase are hot-forged by multi-pass.At this point, copper niobium is multiple
The average-size of niobium phase thickness reaches 2.7 μm in condensation material.
Step 9: copper niobium composite material described in step 8 is carried out milling face and pickling processes, in pickling, dehydration and dry
The rib length of copper niobium composite material Wei not 75mm, 296mm and 390mm afterwards.Cold rolling is carried out to copper niobium composite material, roll reduction is
73mm, the corresponding reduction ratio that rolls are greater than 97.3%, obtain the copper niobium composite board with a thickness of 2mm.At this point, niobium phase ruler in material
Very little in the average thickness for rolling face normal direction is 78nm, and according to the measurement result of SEM-EBSD method, the KAM value for rolling face is 2.8.
Step 10: copper niobium composite board described in step 9 is subjected to pickling processes, and after pickling, dehydration and drying, system
At copper niobium composite finished product.At this point, Tensile strength is 814MPa, conductivity 79.4%IACS.
Embodiment 2
The preparation of Cu-12wt%Nb composite board:
As shown in Figure 1, content of niobium is the preparation of the copper niobium composite board of 12wt%, specifically implement according to the following steps:
Step 1: processing multiple groups circular hole on casting mould inner wall front, circular hole is arranged in array.Circularhole diameter is 2.1mm, deep
Degree is 6mm, and two pitchs of holes are 2.9mm, and the minimum range of circular hole Kong Xinyu mold left side is 52mm.
Step 2: being 2mm by diameter, length is niobium stick totally 6400 of 70mm, and quality is 12.06 kilograms, is embedded in mold
In circular hole, and die assembly is completed.Mold cavity be it is rectangular, type chamber height, length and width be respectively 560mm, 460mm and
65mm。
Step 3: fine copper is packed into graphite crucible, and it is put into vacuum induction melting furnace.It will be in vacuum induction melting furnace
Vacuum degree is reduced to 5.8 × 10-2Pa is subsequently passed argon gas.Metallic copper is melted under an argon atmosphere, smelting temperature is 1400 DEG C.
Cast gate is close to mold left side, and molten metal copper liquid is being kept the temperature after ten minutes, in mold left side injection mold.To gold
After belonging to liquid cooling, ingot casting and mold are taken out.After removing mold, the rectangular billet of copper niobium composite material is obtained.
Step 4: copper niobium composite material billet described in step 3 is carried out crop end and milling face, surface oxide layer is eliminated,
Cut off the extra fine copper in side, obtain height, length and width be respectively 400mm, 400mm and 60mm the compound square billet of copper niobium；
Wherein the content of niobium is 10.34 kilograms；The content of copper is 74.7 kilograms.
Step 5: copper niobium composite material billet described in step 4 is put into the heating furnace inside holding 0.5h that temperature is 900 DEG C.
Step 6: copper niobium composite material described in step 5 is hot-forged, material temperature in hot forging process is greater than 450
DEG C, when temperature reaches 450 DEG C, continue hot forging process after material is put into 800 DEG C of heat preservation 0.5h.Copper niobium composite material after hot forging
Length foreshortens to about 80mm by 400mm, and height still keeps 400mm, and width rises to about 300mm, copper niobium composite material by 60mm
With niobium mandrel to the strain of parallel direction be 1.6.
Step 7: being hot-forged after copper niobium composite material described in step 6 is put into 750 DEG C of heat preservation 1h, material had been hot-forged
Temperature should be greater than 450 DEG C in journey, when temperature reaches 450 DEG C, continue hot forging process after material is put into 750 DEG C of heat preservation 0.5h.Copper
After the hot forging of niobium composite material, the long 300mm that rises to by 80mm of the first rib, the second rib is long to foreshorten to 80mm, third by 400mm
Rib is long to rise to 400mm by 300mm, and material is in the normal strain being parallel on the long direction of the shortest edge up to 1.32.
Step 8: repeating operation 31 times of step 7, refinement copper phase and niobium phase are hot-forged by multi-pass.At this point, copper niobium is multiple
The average-size of niobium phase thickness reaches 2.1 μm in condensation material.
Step 9: copper niobium composite material described in step 8 is carried out milling face and pickling processes, in pickling, dehydration and dry
The rib length of copper niobium composite material Wei not 75mm, 296mm and 390mm afterwards.Cold rolling is carried out to copper niobium composite material, roll reduction is
73mm, the corresponding reduction ratio that rolls are greater than 97.3%, obtain the copper niobium composite board with a thickness of 1mm.At this point, niobium phase ruler in material
Very little in the average thickness for rolling face normal direction is 62nm, and according to the measurement result of SEM-EBSD method, the KAM value for rolling face is 2.9.
Step 10: copper niobium composite board described in step 9 is subjected to pickling processes, and after pickling, dehydration and drying, system
At copper niobium composite finished product.At this point, the tensile strength of copper niobium composite board is 926MPa, conductivity 76.5%IACS.
Embodiment 3
The preparation of Cu-14wt%Nb composite board:
As shown in Figure 1, content of niobium is the preparation of the copper niobium composite board of 14wt%, specifically implement according to the following steps:
Step 1: processing multiple groups circular hole on casting mould inner wall front, circular hole is arranged in array.Circularhole diameter is 2.7mm, deep
Degree is 6mm, and two pitchs of holes are 3.3mm, and the minimum range of circular hole Kong Xinyu mold left side is 52mm.
Step 2: being 2.6mm by diameter, length is niobium stick totally 4356 of 70mm, and quality is 13.87 kilograms, is embedded in mould
Have in circular hole, and die assembly is completed.Mold cavity be it is rectangular, type chamber height, length and width are respectively 560mm, 460mm
And 65mm.
Step 3: fine copper is packed into graphite crucible, and it is put into vacuum induction melting furnace.It will be in vacuum induction melting furnace
Vacuum degree is reduced to 5.8 × 10-2Pa is subsequently passed argon gas.Metallic copper is melted under an argon atmosphere, smelting temperature 1400
℃.Cast gate is close to mold left side, and molten metal copper liquid is being kept the temperature after ten minutes, in mold left side injection mold.
After metal liquid is cooling, ingot casting and mold are taken out.After removing mold, the rectangular billet of copper niobium composite material is obtained.
Step 4: copper niobium composite material billet described in step 3 is carried out crop end and milling face, surface oxide layer is eliminated,
Cut off the extra fine copper in side, obtain height, length and width be respectively 400mm, 400mm and 60mm the compound square billet of copper niobium；
Wherein the content of niobium is 11.89 kilograms；The content of copper is 73.09 kilograms.
Step 5: copper niobium composite material billet described in step 4 is put into the heating furnace inside holding 0.5h that temperature is 900 DEG C.
Step 6: copper niobium composite material described in step 5 is hot-forged, material temperature in hot forging process is greater than 450
DEG C, when temperature reaches 450 DEG C, continue hot forging process after material is put into 800 DEG C of heat preservation 0.5h.Copper niobium composite material after hot forging
Length foreshortens to about 80mm by 400mm, and height still keeps 400mm, and width rises to about 300mm, copper niobium composite material by 60mm
With niobium mandrel to the strain of parallel direction be 1.6.
Step 7: being hot-forged after copper niobium composite material described in step 6 is put into 750 DEG C of heat preservation 1h, material had been hot-forged
Temperature should be greater than 450 DEG C in journey, when temperature reaches 450 DEG C, continue hot forging process after material is put into 750 DEG C of heat preservation 0.5h.Copper
After the hot forging of niobium composite material, the long 300mm that rises to by 80mm of the first rib, the second rib is long to foreshorten to 80mm, third rib by 400mm
Long to rise to 400mm by 300mm, material is in the normal strain being parallel on the long direction of the shortest edge up to 1.32.
Step 8: repeating operation 31 times of step 7, refinement copper phase and niobium phase are hot-forged by multi-pass.At this point, copper niobium is multiple
The average-size of niobium phase thickness reaches 1.9 μm in condensation material.
Step 9: copper niobium composite material described in step 8 is carried out milling face and pickling processes, in pickling, dehydration and dry
The rib length of copper niobium composite material Wei not 75mm, 296mm and 390mm afterwards.Cold rolling is carried out to copper niobium composite material, roll reduction is
74mm, the corresponding reduction ratio that rolls are greater than 98.6%, obtain the copper niobium composite board with a thickness of 1mm.At this point, niobium phase ruler in material
Very little in the average thickness for rolling face normal direction is 38nm, and according to the measurement result of SEM-EBSD method, the KAM value for rolling face is 3.2.
Step 10: copper niobium composite board described in step 9 is subjected to pickling processes, and after pickling, dehydration and drying, system
At copper niobium composite finished product.At this point, the tensile strength of copper niobium composite board is 958MPa, conductivity 74.2%IACS.
Embodiment 4
The preparation of Cu-17wt%Nb composite board:
As shown in Figure 1, content of niobium is the preparation of the copper niobium composite board of 14wt%, specifically implement according to the following steps:
Step 1: processing multiple groups circular hole on casting mould inner wall front, circular hole is arranged in array.Circularhole diameter is 2.5mm, deep
Degree is 6mm, and two pitchs of holes are 2.5mm, and the minimum range of circular hole Kong Xinyu mold left side is 52mm.
Step 2: being 2.4mm by diameter, length is niobium stick totally 6400 of 70mm, and quality is 17.37 kilograms, is embedded in mould
Have in circular hole, and die assembly is completed.Mold cavity be it is rectangular, type chamber height, length and width are respectively 560mm, 460mm
And 65mm.
Step 3: fine copper is packed into graphite crucible, and it is put into vacuum induction melting furnace.It will be in vacuum induction melting furnace
Vacuum degree is reduced to 5.8 × 10-2Pa is subsequently passed argon gas.Metallic copper is melted under an argon atmosphere, smelting temperature 1450
℃.Cast gate is close to mold left side, and molten metal copper liquid is being kept the temperature after ten minutes, in mold left side injection mold.
After metal liquid is cooling, ingot casting and mold are taken out.After removing mold, the rectangular billet of copper niobium composite material is obtained.
Step 4: copper niobium composite material billet described in step 3 is carried out crop end and milling face, surface oxide layer is eliminated,
Cut off the extra fine copper in side, obtain height, length and width be respectively 400mm, 400mm and 60mm the compound square billet of copper niobium；
Wherein the content of niobium is 14.89 kilograms；The content of copper is 69.98 kilograms.
Step 5: copper niobium composite material billet described in step 4 is put into the heating furnace inside holding 0.5h that temperature is 900 DEG C.
Step 6: copper niobium composite material described in step 5 is hot-forged, material temperature in hot forging process is greater than 450
DEG C, when temperature reaches 450 DEG C, continue hot forging process after material is put into 800 DEG C of heat preservation 0.5h.Copper niobium composite material after hot forging
Length foreshortens to about 80mm by 400mm, and height still keeps 400mm, and width rises to about 300mm, copper niobium composite material by 60mm
With niobium mandrel to the strain of parallel direction be 1.6.
Step 7: being hot-forged after copper niobium composite material described in step 6 is put into 750 DEG C of heat preservation 1h, material had been hot-forged
Temperature should be greater than 450 DEG C in journey, when temperature reaches 450 DEG C, continue hot forging process after material is put into 750 DEG C of heat preservation 0.5h.Copper
After the hot forging of niobium composite material, the long 300mm that rises to by 80mm of the first rib, the second rib is long to foreshorten to 80mm, third rib by 400mm
Long to rise to 400mm by 300mm, material is in the normal strain being parallel on the long direction of the shortest edge up to 1.32.
Step 8: repeating operation 34 times of step 7, refinement copper phase and niobium phase are hot-forged by multi-pass.At this point, copper niobium is multiple
The average-size of niobium phase thickness reaches 1.5 μm in condensation material.
Step 9: copper niobium composite material described in step 8 is carried out milling face and pickling processes, in pickling, dehydration and dry
The rib length of copper niobium composite material Wei not 75mm, 296mm and 390mm afterwards.Cold rolling is carried out to copper niobium composite material, roll reduction is
74mm, the corresponding reduction ratio that rolls are greater than 98.6%, obtain the copper niobium composite board with a thickness of 1mm.At this point, niobium phase ruler in material
Very little in the average thickness for rolling face normal direction is 24nm, and according to the measurement result of SEM-EBSD method, the KAM value for rolling face is 3.3.
Step 10: copper niobium composite board described in step 9 is subjected to pickling processes, and after pickling, dehydration and drying, system
At copper niobium composite finished product.At this point, the tensile strength of copper niobium composite board is 1041MPa, conductivity 68.7%IACS.
Above-mentioned example is only intended to illustrate the present invention, and in addition to this, also there are many different embodiments, and these are implemented
Mode be all those skilled in the art after comprehension inventive concept it is also envisioned that therefore, will not enumerate herein.
Claims (6)
1. a kind of preparation method of copper niobium composite material, which comprises the following steps:
Step 1: production mold, the mold is made of the first component and the docking of second component level, the side of mold inner-cavity by
Channel is poured up to being arranged with；The area for removing casting channel part is effective area, if uniformly distributed in the effective area
Dry niobium stick mounting hole, the niobium in niobium stick alloy are mounted in the niobium stick mounting hole in the form of niobium stick；
Step 2: niobium stick made of several pure niobiums is horizontally inserted into the niobium stick mounting hole, the first component with it is described
The height and width of second component composition mold inner-cavity are all larger than 5 times of thickness or more of mold；
Step 3: fine copper is packed into graphite crucible, and it is put into vacuum induction melting furnace, by the vacuum in vacuum induction melting furnace
Degree should be reduced to 6.0 × 10-2Pa or less；Be filled with protective gas, melt copper under protective atmosphere, smelting temperature at 1200 DEG C extremely
Between 1450 DEG C；Heat preservation 5 to 10 minutes injects mold inner-cavity from the casting channel of mold；Billet is formed after cooling；
Step 4: the billet is carried out crop end and milling face, surface oxide layer is eliminated, the extra fine copper in excision side obtains
The compound square billet of copper niobium；
0.5 to 1 hour is kept the temperature Step 5: the compound square billet of copper niobium is put into 700 DEG C to 800 DEG C of heating furnace；
Step 6: being hot-forged to the compound square billet of copper niobium, hot forging temperature is not less than 450 DEG C；After hot forging, with niobium mandrel to flat
The strain of line direction is greater than 1.5；
Step 7: the compound square billet of copper niobium is put into keep the temperature 0.5 to 1 hour in 800 DEG C to 900 DEG C of heating furnace after carry out heat
Forging；It is greater than 1.2 in the normal strain being parallel on the long direction of the shortest edge；
Step 8: step 7 at least repeats 28 times；
Step 9: the compound square billet of copper niobium is carried out milling face and pickling processes, after pickling, dehydration and drying；Cold rolling is carried out,
It rolls reduction ratio and is greater than 97.3%, obtain copper niobium composite board.
2. the preparation method of copper niobium composite material as described in claim 1, which is characterized in that the diameter of the niobium stick mounting hole
For 0.5-4mm, depth 5-10mm, two pitchs of holes are greater than 2mm.
3. the preparation method of copper niobium composite material as described in claim 1, which is characterized in that the width in the casting channel is big
In 40mm.
4. the preparation method of copper niobium composite material as described in claim 1, which is characterized in that the quality of the pure niobium and fine copper
Purity is not less than 99.9%.
5. the preparation method of copper niobium composite material as described in claim 1, which is characterized in that material in step 6 and step 7
Temperature is greater than 450 DEG C, when temperature is at 450-500 DEG C, after material is put into 700-800 DEG C of heat preservation 0.5h in entire hot forging process
Continue hot forging process.
6. the preparation method of copper niobium composite material as described in claim 1, which is characterized in that niobium in the copper niobium composite material
Mass percent between 10% to 20, surplus is copper and the impurity that not can be removed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910862326.8A CN110465643B (en) | 2019-09-12 | 2019-09-12 | Preparation method of copper-niobium composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910862326.8A CN110465643B (en) | 2019-09-12 | 2019-09-12 | Preparation method of copper-niobium composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110465643A true CN110465643A (en) | 2019-11-19 |
| CN110465643B CN110465643B (en) | 2021-02-26 |
Family
ID=68515657
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910862326.8A Active CN110465643B (en) | 2019-09-12 | 2019-09-12 | Preparation method of copper-niobium composite material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110465643B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111331104A (en) * | 2020-03-20 | 2020-06-26 | 辽宁科技大学 | Preparation method of fine-grain homogeneous compact large-scale metal plate blank or plate |
| CN112270078A (en) * | 2020-10-16 | 2021-01-26 | 西南科技大学 | Method for predicting depth of multi-pass nano scratches of brittle material |
| CN113385895A (en) * | 2020-09-29 | 2021-09-14 | 中国科学院近代物理研究所 | High-stability niobium-based superconducting accelerating cavity and preparation method thereof |
| CN113969364A (en) * | 2021-09-10 | 2022-01-25 | 中南大学 | High-strength high-conductivity copper-niobium alloy and preparation method thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2407764A1 (en) * | 1974-02-19 | 1975-08-28 | Kabel Metallwerke Ghh | METHOD OF MANUFACTURING A STABILIZED SUPRAL CONDUCTOR |
| JPS61115659A (en) * | 1984-11-12 | 1986-06-03 | Toyota Motor Corp | Production of partially alloyed casting |
| JPS61195738A (en) * | 1985-02-25 | 1986-08-30 | Furukawa Electric Co Ltd:The | Production of composite material for compound superconductive wire |
| JPS62263956A (en) * | 1986-05-08 | 1987-11-16 | Mitsubishi Heavy Ind Ltd | Manufacture of hollow vessel with two-layer structure |
| US4708847A (en) * | 1983-07-28 | 1987-11-24 | Toyota Jidosha Kabushiki Kaisha | Method for alloying substances |
| CN1045049A (en) * | 1988-02-22 | 1990-09-05 | 蒂玛夫公司 | A kind of method that between material product and foundry goods, obtains metallurgical, bond |
| JPH11250747A (en) * | 1998-02-27 | 1999-09-17 | Kobe Steel Ltd | Manufacture of nb3sn based superconducting wire |
| CN1816401A (en) * | 2003-07-02 | 2006-08-09 | Ati资产公司 | Method for producing metal fibers |
| CN106676313A (en) * | 2016-12-28 | 2017-05-17 | 北京有色金属研究总院 | Preparation method of high-intensity and high-conductivity Cu-Nb alloy billet |
| CN107350304A (en) * | 2017-06-26 | 2017-11-17 | 江西理工大学 | A kind of high-strength copper niobium composite wire and preparation method thereof |
| CN109022860A (en) * | 2018-09-19 | 2018-12-18 | 濮阳市华信技术服务有限公司 | A kind of preparation method of high-strength high-conductivity Cu-Ag alloy |
-
2019
- 2019-09-12 CN CN201910862326.8A patent/CN110465643B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2407764A1 (en) * | 1974-02-19 | 1975-08-28 | Kabel Metallwerke Ghh | METHOD OF MANUFACTURING A STABILIZED SUPRAL CONDUCTOR |
| US4708847A (en) * | 1983-07-28 | 1987-11-24 | Toyota Jidosha Kabushiki Kaisha | Method for alloying substances |
| JPS61115659A (en) * | 1984-11-12 | 1986-06-03 | Toyota Motor Corp | Production of partially alloyed casting |
| JPS61195738A (en) * | 1985-02-25 | 1986-08-30 | Furukawa Electric Co Ltd:The | Production of composite material for compound superconductive wire |
| JPS62263956A (en) * | 1986-05-08 | 1987-11-16 | Mitsubishi Heavy Ind Ltd | Manufacture of hollow vessel with two-layer structure |
| CN1045049A (en) * | 1988-02-22 | 1990-09-05 | 蒂玛夫公司 | A kind of method that between material product and foundry goods, obtains metallurgical, bond |
| JPH11250747A (en) * | 1998-02-27 | 1999-09-17 | Kobe Steel Ltd | Manufacture of nb3sn based superconducting wire |
| CN1816401A (en) * | 2003-07-02 | 2006-08-09 | Ati资产公司 | Method for producing metal fibers |
| CN106676313A (en) * | 2016-12-28 | 2017-05-17 | 北京有色金属研究总院 | Preparation method of high-intensity and high-conductivity Cu-Nb alloy billet |
| CN107350304A (en) * | 2017-06-26 | 2017-11-17 | 江西理工大学 | A kind of high-strength copper niobium composite wire and preparation method thereof |
| CN109022860A (en) * | 2018-09-19 | 2018-12-18 | 濮阳市华信技术服务有限公司 | A kind of preparation method of high-strength high-conductivity Cu-Ag alloy |
Non-Patent Citations (1)
| Title |
|---|
| 罗泽宇等: "累积叠轧Cu/Nb 复合板材在形变与退火过程中的", 《金属热处理》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111331104A (en) * | 2020-03-20 | 2020-06-26 | 辽宁科技大学 | Preparation method of fine-grain homogeneous compact large-scale metal plate blank or plate |
| CN113385895A (en) * | 2020-09-29 | 2021-09-14 | 中国科学院近代物理研究所 | High-stability niobium-based superconducting accelerating cavity and preparation method thereof |
| CN113385895B (en) * | 2020-09-29 | 2022-04-26 | 中国科学院近代物理研究所 | High-stability niobium-based superconducting accelerating cavity and preparation method thereof |
| CN112270078A (en) * | 2020-10-16 | 2021-01-26 | 西南科技大学 | Method for predicting depth of multi-pass nano scratches of brittle material |
| CN112270078B (en) * | 2020-10-16 | 2022-02-15 | 西南科技大学 | Method for predicting depth of multi-pass nano scratches of brittle material |
| CN113969364A (en) * | 2021-09-10 | 2022-01-25 | 中南大学 | High-strength high-conductivity copper-niobium alloy and preparation method thereof |
| CN113969364B (en) * | 2021-09-10 | 2022-05-03 | 中南大学 | High-strength high-conductivity copper-niobium alloy and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110465643B (en) | 2021-02-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110465643A (en) | A kind of preparation method of copper niobium composite material | |
| RU2490350C2 (en) | METHOD FOR OBTAINING BASIC β-γ-TiAl-ALLOY | |
| CN112481513B (en) | Process for preparing copper-chromium alloy electrical contact consumable electrode by using CuCr metal powder | |
| CN106756372B (en) | A kind of high-performance aluminizing-preparation method of rare earth alloy and its product of preparation | |
| CN107739878B (en) | A kind of anti-softening copper alloy of high-strength highly-conductive and preparation method thereof | |
| KR101782202B1 (en) | High-purity titanium ingots, manufacturing method therefor, and titanium sputtering target | |
| CN105274365A (en) | Titanium alloy preparation technology | |
| JP2001240949A (en) | Method of manufacturing for worked billet of high- purity copper having fine crystal grain | |
| CN103526038B (en) | A kind of high-strength high-plasticity TWIP steel esr production method | |
| CN108796304A (en) | A kind of γ-TiAl prealloys gas-atomized powder electrode bar and preparation method thereof | |
| CN103938002B (en) | A kind of Cu-Cr-Zr alloy casting rod reduces the vacuum melting technique of segregation | |
| JP2021529262A (en) | High hardness and high conductivity Cu-Ag-Sc alloy and its manufacturing method | |
| CN106498226A (en) | A kind of photomultiplier tube dynode is with high beallon preparation method | |
| CN105803257A (en) | Method for improving liquid-state fluidity of TiAl-Nb alloy | |
| CN108866365A (en) | A kind of high-quality titanium aluminium pre-alloyed powder electrode preparation method | |
| CN113134608A (en) | Device and method for preparing nickel-based high-temperature alloy blank by pulse current auxiliary sintering | |
| CN102392205A (en) | Method for preparing precision copper part | |
| CN106957986A (en) | A kind of high-ductility magnetostriction materials and preparation method thereof | |
| CN106756207A (en) | A kind of short process making method of high-strength highly-conductive deformation Cu Cr Ag in-situ composites | |
| CN107326225A (en) | Aluminium alloy and preparation method thereof, target material assembly and its manufacture method | |
| JP4512542B2 (en) | Flotation melting casting method and water-cooled crucible used in the casting method | |
| CN101941066A (en) | Ceramic casting mold applied to metal casting under electric field treatment and method for casting titanium aluminum-based alloy by using same | |
| CN102286710B (en) | Method for preparing alloy semi-solid forming plate blanks by casting and rolling dual control method | |
| CN108165814A (en) | A kind of carbon microalloy Cu-Cr based materials and preparation method thereof | |
| CN109536817B (en) | Tungsten high-entropy alloy with armor-piercing self-sharpening effect and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |