CN107475559B - A kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy and preparation method thereof - Google Patents
A kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—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
Abstract
The present invention provides a kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy and preparation method thereof.The chrome zirconium copper alloy includes: 9~14% chromium, 0.24~0.6% zirconium, 0.006~0.019% magnesium, 0.008~0.13% X, and surplus is copper；X is any one or several in selenium, nickel, silicon and iron.Preparation method are as follows: raw material shove charge；It vacuumizes, is filled with protective gas, heat up melting copper；Continue to heat up, melting chromium；Zirconium is added in crucible, after zirconium is melting down, when being cooled to melting down melt epidermis and starting solidification, is vacuumized, and after filling protective gas, it is melting down again to be warming up to melt, cools down, casting, cooling is come out of the stove.Pass through reasonable design of alloy, improve chromium constituent content, and other components and its content are adjusted, obtain the copper alloy of high-intensitive (850~950MPa), highly conductive (82%~90%IACS), thermal stability good (610~630 DEG C of softening temperature).
Description
Technical field
The invention belongs to technical field of alloy material, be related to one kind be suitable for intensity, electric conductivity, thermal stability and have it is very high
It is required that high-intensitive, highly conductive, high thermal stability copper alloy, and in particular to a kind of high-strength highly-conductive high thermal stability chromium-zirconium-copper is closed
Gold and preparation method thereof.
Background technique
Chromium-zirconium-copper series copper alloy is a kind of widely used high conduction performance alloy, is now widely used for spiral bullet
The industrial circles such as spring fingertip, circuit lead frame, electric car and electric locomotive contact line, are mainly characterized by with higher
Conductivity, but low strength.
Screw-contact is the novel movable electrical contact contact of one kind just occurred in recent years.It is conventionally used to preparation spiral bullet
The chrome zirconium copper alloy intensity of spring fingertip is 400~500MPa, and electric conductivity is 75~80%IACS, compared to other two kinds of spiral shells of market
Revolve spring touch finger Cu alloy material CuBe2(1100~1580MPa of intensity, 18~24%IACS of electric conductivity, beryllium are toxic), CuCo2Be
(750~970MPa of intensity, 58~62%IACS of electric conductivity, beryllium are toxic), chromium-zirconium-copper shows good conductivity, free of contamination performance
Feature, but the bottleneck low there are intensity, since the chromium-zirconium-copper silk material that the current country of technical restriction uses largely is dependent at present
Import, price be also it is most expensive in three kinds of silk materials, more expensive than domestic beryllium copper about 20%, be 3 times of domestic chromium-zirconium-copper.
Lead frame Cu alloy material is one of chief component of integrated circuit, plays connection transmission telecommunications number, heat dissipation
Etc. functions.As integrated circuit is to extensive and ultra-large development, it is more than 600MPa that lead frame copper strip, which requires tensile strength,
Conductivity is greater than 80%IACS, and anti-softening temperature is greater than 527 DEG C.Current developed lead frame acid bronze alloy mainly has
CuFeP system, CuNiSi system, CuCrZr system etc., though these alloy materials are able to satisfy certain demand, there are still overall performances not
The disadvantages of good.
The development of long pulse high-intensity magnetic field technology and high-speed electric railway, to magnetic field conductors and power contacts wire material performance
It puts forward new requirements, needs the good combination of high strength & high electric-conduction and high-termal conductivity.Its performance requirement is tensile strength >
700MPa, conductivity > 75%, using temperature at 300 DEG C tensile strength rate of descent below 10%.
105543540 A of Chinese patent CN discloses a kind of chrome zirconium copper alloy and preparation method thereof, such alloy is tradition
Low chromium (0.7~2.0%) chrome zirconium copper alloy, tensile strength > 520MPa, conductivity >=90%IACS, 350 DEG C of elevated temperature tensiles
Intensity > 390MPa, though conductivity is good, tensile strength and high-temperature stability are relatively low.Chinese patent CN102912178A is disclosed
A kind of high-strength highly-conductive rare-earth copper alloy and preparation method thereof, such alloy is that traditional low chromium (0.2~1.0%) Cu-RE closes
Gold, tensile strength > 550MPa, hardness > 150HV, 450 DEG C of conductivity > 80%IACS, softening temperature >, though conductivity
It is good, but hardness, tensile strength and high-temperature stability are relatively low.A kind of copper-based in-situ disclosed in Chinese patent CN101225486A is compound
Material and preparation method thereof, alloy include 6~16% chromium；0.02~0.2% zirconium, remaining be copper.Directly add when its melting
Add zirconium simple substance, and mixed smelting is carried out simultaneously to three kinds of chromium, zirconium, copper simple substance elements, is first hot-forged the work being dissolved afterwards to ingot casting later
Skill route, gained chromium-zirconium-copper Tensile strength be 850~1300MPa, 70~80%IACS of conductivity, softening temperature 500~
550 DEG C, though intensity is high, conductivity and softening temperature be not good enough.
It therefore is to be well positioned to meet screw-contact, super large-scale integration lead frame, flash high-strength magnetic
For the industrial circles such as field and high-speed electric railway to the rigors of Cu alloy material, it is really necessary to provide a kind of high-strength highly-conductive height
Thermal stability chrome zirconium copper alloy and preparation method thereof.
Summary of the invention
Aiming at the problems existing in the prior art, the present invention provide a kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy and
Preparation method, this material have both the advantages that high strength and high conductivity, thermal stability are good, pollution-free, significantly improve chromium-zirconium-copper conjunction
The comprehensive performance of golden material.
The present invention is to be achieved through the following technical solutions:
A kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy includes by weight percentage following component: 9~14%
Chromium, 0.24~0.6% zirconium, 0.006~0.019% magnesium, 0.008~0.13% X, surplus is copper；X is selenium, nickel, silicon
Any one or more of with iron.
Preferably, tensile strength is 850~950MPa；Conductivity is 82%~90%IACS；Microhardness be 170~
230HV0.1；Softening temperature is 610~630 DEG C.
A kind of preparation method of high-strength highly-conductive high thermal stability chrome zirconium copper alloy described in claim 1, includes the following steps:
Step 1, raw material shove charge；Any one or more of chromium, copper and magnesium and selenium, nickel, silicon and iron are placed in together
In crucible；And zirconium and crucible are respectively placed in furnace；
Step 2, temperature being risen to 100~200 DEG C, heating crucible vacuumizes, and is filled with protective gas, it is warming up to 1150~
1200 DEG C, 23~30min of melting copper, stand 5~10min；
Step 3,1510~1580 DEG C are continuously heating to, melting down to chromium, heat preservation stands 5~10min；
Step 4, by zirconium be added crucible in, after zirconium is melting down, be cooled to melting down melt epidermis start solidification when, vacuumize,
And heat up after filling protective gas, while electromagnetic agitation to melt it is melting down again after, melt is poured when being cooled to 1300~1400 DEG C
Enter in the mold in furnace, obtains slab；
Step 5,400~500 DEG C are furnace-cooled in protective gas atmosphere, slab is come out of the stove, and water cooling to room temperature obtains ingot casting.
Preferably, copper selects oxygen-free copper in step 1, before step 1 further includes the cleaning step of oxygen-free copper, specially will
Oxygen-free copper is placed in cleaner for metal, brushes surface and oil contaminant with cotton, after with clear water clean and with compressor gun dry up anaerobic
Copper；The cleaner for metal is by powdery metal cleaning agent with 35~40 DEG C of hot water with 1:(45~50) mass ratio is formulated.
Preferably, in step 2, reach (1~7) × 10 to vacuum degree-2After Pa, argon gas is filled with to 0.01~0.04MPa.
Preferably, in step 4, melting down melt epidermis starts to be evacuated to 2~2.5Pa when solidification, and applying argon gas is to 0.05
It heats up after~0.08MPa.
Preferably, further include step 6 homogenizing annealing: the ingot casting that step 5 is obtained is heated to 910~970 DEG C, heat preservation
1.5~3h.
Further, further include that step 7 water seal squeezes: the ingot casting after step 6 homogenizing annealing is subjected to water seal extruding, water
Hardening heat is 840~930 DEG C when envelope squeezes, and extrusion deformation degree 62%~78% obtains bar stock.
Further, further include step 8 cold rolling: the bar stock that step 7 is obtained carries out cold rolling.
Further, further include step 9 drawing deformation and ageing treatment: the bar stock that step 8 is obtained carries out drawing deformation,
Deflection is 15%~50%, and 0.5~1.5h of heat preservation carries out ageing treatment at being later 460~540 DEG C in annealing temperature.
Compared with prior art, the invention has the following beneficial technical effects:
The present invention improves the content of chromium component by reasonable design of alloy, and adjusts other components and its content,
Acquisition high-intensitive (850~950MPa), highly conductive (82%~90%IACS), thermal stability are good (610~630 DEG C of softening temperature)
Copper alloy be able to satisfy helical spring touching particularly suitable for the occasion having high requirements to intensity, electric conductivity and thermal stability
Rigors of the industrial circles such as finger, lead frame, electric car and electric locomotive contact line to copper alloy performance.
In the present invention, chrome zirconium copper alloy material use original position vacuum casting technique preparation, preferred alloy smelting technology and at
Type technology, stratification melting realize that copper, chromium and zirconium distinguish the mesh of melting by the design of temperature gradient and raw material adding manner
, the advantages that stock utilization is high, scaling loss is small；Gained chrome zirconium copper alloy material segregation-free, microstructure is uniform, comprehensive performance
It is good, it can be used for a variety of industrial circles.While the Cu alloy material materials are simple, low cost, concise in technology, environmental nonpollution is comprehensive
It is good to close performance, cost performance is high, is suitble to large-scale industrial production, can break import monopolies, to electric power, electronics, electric appliance equipment and device
The high performance of part serves to spur, and will generate considerable economic benefit.
Specific embodiment
Embodiments of the present invention are described in further detail below:
A kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy includes following components in percentage by weight: chromium 9~14%,
Zirconium 0.24~0.6%, magnesium 0.006~0.019%, X 0.008~0.13%, surplus are copper；X is appointing in selenium, nickel, silicon and iron
It is one or more of.
The high-strength highly-conductive high thermal stability chrome zirconium copper alloy, tensile strength be 850~950MPa, conductivity be 82%~
90%IACS, microhardness are 170~230HV0.1, softening temperature is 610~630 DEG C.
The preparation method of the high-strength highly-conductive high thermal stability chrome zirconium copper alloy, comprising the following steps:
(1) melting:
1) copper being placed in by powdery metal cleaning agent with 35~40 DEG C of hot water with 1:(45~50) mass ratio is formulated
Metal cleaning solution in, brush surface and oil contaminant with cotton, after with clear water clean and with compressor gun dry up copper.
2) raw material shove charge: taking out after crucible is preheated to 80~110 DEG C in resistance furnace, by load weighted chromium powder copper
Foil wraps up any one or more of copper and selenium, nickel, silicon and the iron for being placed in crucible bottom, and being put into magnesium grain and step 1)；Afterwards
The copper-clad for wrapping up zirconium powder is hung on copper wire and is smash on material bar；It is placed in furnace body by crucible and after assembling the mold of riser, envelope
Furnace.
3) 100~200 DEG C are warming up to, heating crucible vacuumizes degasification, reaches (1~7) × 10 to vacuum degree-2After Pa, fill
Enter argon gas and be warming up to 1150~1200 DEG C, 23~30min of melting copper to 0.01-0.04MPa, and stands 5~10min.
4) 1510~1580 DEG C are continuously heating to, melting down to chromium, heat preservation stands 5~10min.
5) zirconium powder smash on material bar in step 2) is added in crucible, after zirconium is melting down, is cooled to melting down melt epidermis and starts
Solidification, is evacuated to 2~2.5Pa, and heat up after applying argon gas to 0.05~0.08MPa, while electromagnetic agitation melts again to melt
After clear, melt is poured into mold when being cooled to 1300~1400 DEG C, obtains slab.
6) it is furnace-cooled to 400~500 DEG C under protection of argon gas, slab is come out of the stove, and water cooling to room temperature obtains ingot casting.
(2) homogenizing annealing: the ingot casting that step (1) obtains is heated to 910~970 DEG C, keeps the temperature 1.5~3h.
(3) water seal squeezes: will carry out water seal extruding through the ingot casting after step (2) homogenizing annealing, water seal quenches when squeezing
Temperature is 840~930 DEG C, and extrusion deformation degree 62%~78% obtains bar stock.
(4) cold rolling: cold rolling will be carried out through the bar stock that step (3) obtain, and will reduce interface dimensions.
(5) drawing deformation and stress relief annealing: drawing deformation will be carried out through the bar stock that step (4) obtain, deflection is
15%~50%, 0.5~1.5h of heat preservation carries out ageing treatment at being later 460~540 DEG C in annealing temperature；The drawing deformation
With the method for ageing treatment specifically: first carry out first time drawing deformation, deflection be 18%~25%, temperature be 460~
0.5~1.5h is kept the temperature at 540 DEG C carries out ageing treatment；Then second of drawing deformation is carried out, deflection is 20%~50%,
Temperature is that 0.5~1.5h of heat preservation carries out ageing treatment at 460~540 DEG C；Then third time drawing deformation is carried out, deflection is
15%~30%, 0.5~1.5h of heat preservation carries out ageing treatment at being 460~540 DEG C in temperature, obtains high-strength highly-conductive high heat stability
Property chrome zirconium copper alloy.
Below with reference to embodiment, the invention will be described in further detail:
Embodiment 1
A kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy includes following components in percentage by weight: 9% chromium,
0.3% zirconium, 0.006% magnesium, 0.013% nickel, surplus are copper.
Preparation method are as follows:
(1) melting:
1) industrial Cu-CATH-1 bar is placed in by powdery metal cleaning agent and 35 DEG C of hot water with the preparation of 1:45 mass ratio
Made of in metal cleaning solution, brush surface and oil contaminant with cotton, after cleaned with clear water and to dry up industry with compressor gun high
Pure tough cathode bar.
2) raw material shove charge: taking out after Magnesia crucible is preheated to 100 DEG C in resistance furnace, by load weighted chromium powder copper
Foil package is placed in Magnesia crucible bottom, and is put into the industrial Cu-CATH-1 bar of magnesium grain, nickel and step 1)；It will be wrapped with copper wire afterwards
The copper-clad for wrapping up in zirconium powder, which is hung on, to be smash on material bar；Magnesia crucible and the mold for assembling riser are placed in furnace body, banking vacuumizes.
3) 150 DEG C are warming up to, Magnesia crucible is heated, vacuumizes degasification, reach 5.0 × 10 to vacuum degree-2After Pa, it is filled with argon
For gas to 0.03MPa, temperature rises to 1150 DEG C, melting copper 30min, and stands 10min.
4) 1510 DEG C are continuously heating to, melting down to chromium powder, heat preservation stands 10min.
5) zirconium powder smash on material bar in step 2) is added in Magnesia crucible, after zirconium powder is melting down, is cooled to melting down melt table
Skin starts to solidify, and is evacuated to 2.3Pa, and heat up after applying argon gas to 0.07MPa, while electromagnetic agitation waits for that melt is melting down again
Afterwards, melt is poured into mold when being cooled to 1350 DEG C, obtains slab.
6) it is furnace-cooled to 440 DEG C under protection of argon gas, slab is come out of the stove, and water cooling to room temperature obtains ingot casting.
(2) homogenizing annealing: the ingot casting that step (1) obtains is heated to 920 DEG C, keeps the temperature 1.5h.
(3) water seal squeezes: will carry out water seal extruding through the ingot casting after step (2) homogenizing annealing, water seal quenches when squeezing
Temperature is 850 DEG C, and extrusion deformation degree 62% obtains bar stock.
(4) cold rolling: cold rolling will be carried out through the bar stock that step (3) obtain, and will reduce interface dimensions.
(5) drawing deformation and ageing treatment: first time drawing deformation, deflection will be carried out through the bar stock that step (4) obtain
It is 20%, heat preservation 0.5h carries out ageing treatment at being 480 DEG C in temperature；Then second of drawing deformation is carried out, deflection is
30%, heat preservation 0.5h carries out ageing treatment at being 480 DEG C in temperature；Then progress third time drawing deformation, deflection 20%,
Heat preservation 0.5h carries out ageing treatment at being 480 DEG C in temperature, obtains high-strength highly-conductive high thermal stability chrome zirconium copper alloy, alloy property
It is shown in Table 1.
Embodiment 2
A kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy, comprising by following components in percentage by weight: 10% chromium,
0.24% zirconium, 0.017% magnesium, 0.008% selenium and iron, surplus is copper.
Preparation method are as follows:
(1) melting:
1) industrial Cu-CATH-1 bar is placed in by powdery metal cleaning agent and 38 DEG C of hot water with the preparation of 1:48 mass ratio
Made of in metal cleaning solution, brush surface and oil contaminant with cotton, after cleaned with clear water and to dry up industry with compressor gun high
Pure tough cathode bar.
2) raw material shove charge: taking out after Magnesia crucible is preheated to 80 DEG C in resistance furnace, by load weighted chromium powder copper
Foil package is placed in Magnesia crucible bottom, and is put into the industrial Cu-CATH-1 bar of magnesium grain, selenium, iron and step 1)；After use copper wire
The copper-clad for wrapping up zirconium powder is hung on and is smash on material bar；Magnesia crucible and the mold for assembling riser are placed in furnace body, banking is taken out
Vacuum.
3) it is warming up at 100 DEG C and heats Magnesia crucible, vacuumize degasification, reach 1.0 × 10 to vacuum degree-2After Pa, it is filled with
Argon gas is warming up to 1150 DEG C, melting copper 30min to 0.02MPa, and stands 10min.
4) 1510 DEG C are continuously heating to, melting down to chromium powder, heat preservation stands 10min.
5) zirconium powder smash on material bar in step 2) is added in Magnesia crucible, after zirconium powder is melting down, is cooled to melting down melt table
Skin starts to solidify, and is evacuated to 2.0Pa, and heat up after applying argon gas to 0.08MPa, while electromagnetic agitation waits for that melt is melting down again
Afterwards, melt is poured into mold when being cooled to 1350 DEG C, obtains slab.
6) it is furnace-cooled to 440 DEG C under protection of argon gas, slab is come out of the stove, and water cooling to room temperature obtains ingot casting.
(2) homogenizing annealing: the ingot casting that step (1) obtains is heated to 950 DEG C, keeps the temperature 2h.
(3) water seal squeezes: will carry out water seal extruding through the ingot casting after step (2) homogenizing annealing, water seal quenches when squeezing
Temperature is 880 DEG C, and extrusion deformation degree 68% obtains bar stock.
(4) cold rolling: cold rolling will be carried out through the bar stock that step (3) obtain, and will reduce interface dimensions.
(5) drawing deformation and ageing treatment: first time drawing deformation, deflection will be carried out through the bar stock that step (4) obtain
It is 18%, heat preservation 0.5h carries out ageing treatment at being 460 DEG C in temperature；Then second of drawing deformation is carried out, deflection is
20%, heat preservation 0.5h carries out ageing treatment at being 460 DEG C in temperature；Then progress third time drawing deformation, deflection 15%,
Heat preservation 0.5h carries out ageing treatment at being 460 DEG C in temperature, obtains high-strength highly-conductive high thermal stability chrome zirconium copper alloy, alloy property
It is shown in Table 1.
Embodiment 3
A kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy includes following components in percentage by weight: 12% chromium,
0.24% zirconium, 0.012% magnesium, 0.008% nickel and silicon, surplus is copper.
Preparation method are as follows:
(1) melting:
1) raw material shove charge: taking out after crucible is preheated to 90 DEG C in resistance furnace, by load weighted chromium powder copper foil packet
It wraps up in and is placed in crucible bottom, and be put into magnesium grain, nickel, silicon and copper；The copper-clad for wrapping up zirconium powder is hung on copper wire afterwards and is smash on material bar；
Crucible and the mold for assembling riser are placed in furnace body, banking vacuumizes.
2) temperature is heating crucible at 200 DEG C, vacuumizes degasification, reaches 7.0 × 10 to vacuum degree-2After Pa, it is filled with argon gas
To 0.04MPa, 1160 DEG C, melting copper 25min are warming up to, and stands 8min.
3) 1570 DEG C are continuously heating to, melting down to chromium powder, heat preservation stands 7min.
4) zirconium powder smash on material bar in step 2) is added in crucible, after zirconium powder is melting down, is cooled to melting down melt epidermis and opens
Begin to solidify, be evacuated to 2.5Pa, and heat up after applying argon gas to 0.05MPa, while electromagnetic agitation drops after melt is melting down again
Melt is poured into mold when temperature is to 1400 DEG C, obtains slab.
5) it is furnace-cooled to 500 DEG C under protection of argon gas, slab is come out of the stove, and water cooling to room temperature obtains ingot casting.
(2) homogenizing annealing: the ingot casting that step (1) obtains is heated to 950 DEG C, keeps the temperature 3h.
(3) water seal squeezes: will carry out water seal extruding through the ingot casting after step (2) homogenizing annealing, water seal quenches when squeezing
Temperature is 880 DEG C, and extrusion deformation degree 75% obtains bar stock.
(4) cold rolling: cold rolling will be carried out through the bar stock that step (3) obtain, and will reduce interface dimensions.
(5) drawing deformation and ageing treatment: first time drawing deformation, deflection will be carried out through the bar stock that step (4) obtain
It is 23%, heat preservation 1h carries out ageing treatment at being 520 DEG C in temperature；Then second of drawing deformation is carried out, deflection 50%,
Heat preservation 1h carries out ageing treatment at being 520 DEG C in temperature；Then third time drawing deformation, deflection 23%, in temperature are carried out
It is to keep the temperature 1h at 520 DEG C to carry out ageing treatment, obtains high-strength highly-conductive high thermal stability chrome zirconium copper alloy, alloy property is shown in Table 1.
Embodiment 4
A kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy, comprising by following components in percentage by weight: 14% chromium,
0.3% zirconium, 0.018% magnesium, 0.07% selenium, surplus are copper.
Preparation method are as follows:
(1) melting:
1) oxygen-free copper is placed in the metal being formulated by powdery metal cleaning agent and 40 DEG C of hot water with 1:50 mass ratio
In cleaning solution, brush surface and oil contaminant with cotton, after with clear water clean and with compressor gun dry up oxygen-free copper.
2) raw material shove charge: taking out after crucible is preheated to 110 DEG C in resistance furnace, by load weighted chromium powder copper foil packet
It wraps up in and is placed in crucible bottom, and be put into the oxygen-free copper of magnesium grain, selenium and step 1)；The copper-clad for wrapping up zirconium powder is hung on copper wire afterwards
It smashes on material bar；Crucible and the mold for assembling riser are placed in furnace body, banking vacuumizes.
3) it is warming up to heating crucible at 180 DEG C, vacuumizes degasification, reaches 3.0 × 10 to vacuum degree-2After Pa, it is filled with argon gas
To 0.01MPa, 1200 DEG C, melting copper 28min are warming up to, and stands 8min.
4) 1580 DEG C are continuously heating to, melting down to chromium powder, heat preservation stands 5min.
5) zirconium powder smash on material bar in step 2) is added in crucible, after zirconium powder is melting down, is cooled to melting down melt epidermis and opens
Begin solidification, is evacuated to 2.0Pa, and heat up after applying argon gas to 0.07MPa, while electromagnetic agitation is after melt is melting down again, when
Melt is poured into mold when greenhouse cooling is to 1400 DEG C, obtains slab.
6) it is furnace-cooled to 500 DEG C under protection of argon gas, slab is come out of the stove, and water cooling to room temperature obtains ingot casting.
(2) homogenizing annealing: the ingot casting that step (1) obtains is heated to 970 DEG C, keeps the temperature 1.5h.
(3) water seal squeezes: will carry out water seal extruding through the ingot casting after step (2) homogenizing annealing, water seal quenches when squeezing
Temperature is 930 DEG C, and extrusion deformation degree 78% obtains bar stock.
(4) cold rolling: cold rolling will be carried out through the bar stock that step (3) obtain, and will reduce interface dimensions.
(5) drawing deformation and ageing treatment: first time drawing deformation, deflection will be carried out through the bar stock that step (4) obtain
It is 25%, heat preservation 1.5h carries out ageing treatment at being 540 DEG C in temperature；Then second of drawing deformation is carried out, deflection is
40%, heat preservation 1.5h carries out ageing treatment at being 540 DEG C in temperature；Then progress third time drawing deformation, deflection 25%,
Heat preservation 1.5h carries out ageing treatment at being 540 DEG C in temperature, obtains high-strength highly-conductive high thermal stability chrome zirconium copper alloy, alloy property
It is shown in Table 1.
Embodiment 5
A kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy, comprising by following components in percentage by weight: 10% chromium,
0.6% zirconium, 0.019% magnesium, 0.13% nickel, surplus are copper.
Preparation method are as follows:
(1) melting:
1) Magnesia crucible: being preheated to 90 DEG C or so rear taking-ups by raw material shove charge in resistance furnace, by load weighted chromium powder
It is placed in Magnesia crucible bottom with copper foil package, and is put into magnesium grain and industrial Cu-CATH-1 bar；Zirconium powder will be wrapped up with copper wire afterwards
Copper-clad hang on smash material bar on；Magnesia crucible and the mold for assembling riser are placed in furnace body, banking vacuumizes.
2) it is warming up at 200 DEG C and heats Magnesia crucible, vacuumize degasification, reach 5.0 × 10 to vacuum degree-2After Pa, it is filled with
Argon gas promotes temperature to 1200 DEG C of melting copper 23min to 0.03MPa, and stands 5min.
3) 1565 DEG C are continuously heating to, melting down to chromium powder, heat preservation stands 5min.
4) zirconium powder smash on material bar in step 2) is added in Magnesia crucible, after zirconium powder is melting down, is cooled to melting down melt table
Skin starts to solidify, and is evacuated to 2.3Pa, and heat up after applying argon gas to 0.07MPa, while electromagnetic agitation waits for that melt is melting down again
Afterwards, melt is poured into mold when being cooled to 1300 DEG C, obtains slab.
5) it is furnace-cooled to 400 DEG C under protection of argon gas, slab is come out of the stove, and water cooling to room temperature obtains ingot casting.
(2) homogenizing annealing: the ingot casting that step (1) obtains is heated to 910 DEG C, keeps the temperature 2.5h.
(3) water seal squeezes: will carry out water seal extruding through the ingot casting after step (2) homogenizing annealing, water seal quenches when squeezing
Temperature is 840 DEG C, and extrusion deformation degree 70% obtains bar stock, then through subsequent processing, obtains high-strength highly-conductive high thermal stability chromium-zirconium-copper
Alloy, alloy property are shown in Table 1.
Embodiment 6
A kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy, comprising by following components in percentage by weight: 11% chromium,
0.5% zirconium, 0.008% magnesium, 0.1% silicon and iron, surplus is copper.
Preparation method are as follows:
1) copper is placed in the metal cleaning being formulated by powdery metal cleaning agent and 40 DEG C of hot water with 1:50 mass ratio
In solution, brush surface and oil contaminant with cotton, after with clear water clean and with compressor gun dry up copper.
2) raw material shove charge: taking out after crucible is preheated to 100 DEG C in resistance furnace, by load weighted chromium powder copper foil packet
It wraps up in and is placed in crucible bottom, and be put into the copper of magnesium grain and step 1)；The copper-clad for wrapping up zirconium powder is hung on copper wire afterwards and smashes material bar
On；Crucible and the mold for assembling riser are placed in furnace body, banking vacuumizes.
3) temperature is heating crucible at 150 DEG C, vacuumizes degasification, reaches 5.0 × 10 to vacuum degree-2After Pa, it is filled with argon gas
To 0.03MPa, 1170 DEG C, melting copper 28min are warming up to, and stands 6min.
4) 1530 DEG C are continuously heating to, melting down to chromium powder, heat preservation stands 6min.
5) zirconium powder smash on material bar in step 2) is added in crucible, after zirconium powder is melting down, is cooled to melting down melt epidermis and opens
Begin to solidify, be evacuated to 2.3Pa, and heat up after applying argon gas to 0.07MPa, while electromagnetic agitation drops after melt is melting down again
Melt is poured into mold when temperature is to 1350 DEG C, obtains slab.
6) it is furnace-cooled to 470 DEG C under protection of argon gas, slab is come out of the stove, water cooling to room temperature, then through subsequent processing, obtains high-strength height
High thermal stability chrome zirconium copper alloy is led, alloy property is shown in Table 1.
The high-strength highly-conductive high thermal stability chrome zirconium copper alloy performance that 1 embodiment 1-6 of table is obtained
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
A specific embodiment of the invention is only limitted to this, for those of ordinary skill in the art to which the present invention belongs, is not taking off
Under the premise of from present inventive concept, several simple deduction or replace can also be made, all shall be regarded as belonging to the present invention by institute
Claims of submission determine scope of patent protection.
Claims (6)
1. a kind of preparation method of high-strength highly-conductive high thermal stability chrome zirconium copper alloy, which is characterized in that the high-strength highly-conductive high fever
Stability chrome zirconium copper alloy, by weight percentage, include following component: 9~14% chromium, 0.24~0.6% zirconium,
0.006~0.019% magnesium, 0.008~0.13% X, surplus are copper；X is any one or more of selenium, nickel, silicon and iron；
Described method includes following steps:
Step 1, raw material shove charge；Any one or more of chromium, copper and magnesium and selenium, nickel, silicon and iron are placed in crucible together
In；And zirconium and crucible are respectively placed in furnace；
Step 2, temperature is risen to 100~200 DEG C, heating crucible vacuumizes, and is filled with protective gas, is warming up to 1150~1200
DEG C, 23~30min of melting copper stands 5~10min；
Step 3,1510~1580 DEG C are continuously heating to, melting down to chromium, heat preservation stands 5~10min；
Step 4, by zirconium be added crucible in, after zirconium is melting down, be cooled to melting down melt epidermis start solidification when, vacuumize, and fill
Heat up after protective gas, at the same electromagnetic agitation to melt it is melting down again after, melt is poured into furnace when being cooled to 1300~1400 DEG C
In mold in, obtain slab；
Step 5,400~500 DEG C are furnace-cooled in protective gas atmosphere, slab is come out of the stove, and water cooling to room temperature obtains ingot casting；
Step 6 homogenizing annealing: the ingot casting that step 5 is obtained is heated to 910~970 DEG C, keeps the temperature 1.5~3h；
Step 7 water seal squeezes: the ingot casting after step 6 homogenizing annealing being carried out water seal extruding, hardening heat is when water seal squeezes
840~930 DEG C, extrusion deformation degree 62%~78% obtains bar stock；
Step 8 cold rolling: the bar stock that step 7 is obtained carries out cold rolling；
Step 9 drawing deformation and ageing treatment: the bar stock that step 8 is obtained carries out drawing deformation, and deflection is 15%~50%,
0.5~1.5h of heat preservation carries out ageing treatment at being later 460~540 DEG C in annealing temperature；The drawing deformation and ageing treatment
Method specifically: first carry out first time drawing deformation, deflection be 18%~25%, temperature be 460~540 DEG C at keep the temperature
0.5~1.5h carries out ageing treatment；Then carry out second of drawing deformation, deflection is 20%~50%, temperature be 460~
0.5~1.5h is kept the temperature at 540 DEG C carries out ageing treatment；Then third time drawing deformation is carried out, deflection is 15%~30%,
Temperature is that 0.5~1.5h of heat preservation carries out ageing treatment at 460~540 DEG C, obtains high-strength highly-conductive high thermal stability chrome zirconium copper alloy.
2. a kind of preparation method of high-strength highly-conductive high thermal stability chrome zirconium copper alloy according to claim 1, feature exist
In copper selects oxygen-free copper in step 1, before step 1 further includes the cleaning step of oxygen-free copper, oxygen-free copper is specially placed in gold
Belong to cleaning solution in, brush surface and oil contaminant with cotton, after with clear water clean and with compressor gun dry up oxygen-free copper；The metal is clear
Washing lotion is by powdery metal cleaning agent with 35~40 DEG C of hot water with 1:(45~50) mass ratio is formulated.
3. a kind of preparation method of high-strength highly-conductive high thermal stability chrome zirconium copper alloy according to claim 1, feature exist
In reaching (1~7) × 10 to vacuum degree in step 2-2After Pa, argon gas is filled with to 0.01~0.04MPa.
4. a kind of preparation method of high-strength highly-conductive high thermal stability chrome zirconium copper alloy according to claim 1, feature exist
In in step 4, melting down melt epidermis starts to be evacuated to 2~2.5Pa when solidification, and rises after applying argon gas to 0.05~0.08MPa
Temperature.
5. a kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy obtained based on claim 1 the method, which is characterized in that
By weight percentage, comprising following component: 9~14% chromium, 0.24~0.6% zirconium, 0.006~0.019% magnesium,
0.008~0.13% X, surplus are copper；X is any one or more of selenium, nickel, silicon and iron.
6. a kind of high-strength highly-conductive high thermal stability chrome zirconium copper alloy according to claim 5, which is characterized in that tensile strength
For 850~950MPa；Conductivity is 82%~90%IACS；Microhardness is 170~230HV0.1；Softening temperature be 610~
630℃。
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