CN108057732B - A kind of preparation method of dispersion-strengthened Cu and oxygen-free copper composite bar - Google Patents
A kind of preparation method of dispersion-strengthened Cu and oxygen-free copper composite bar Download PDFInfo
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- CN108057732B CN108057732B CN201711270364.1A CN201711270364A CN108057732B CN 108057732 B CN108057732 B CN 108057732B CN 201711270364 A CN201711270364 A CN 201711270364A CN 108057732 B CN108057732 B CN 108057732B
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- 239000010949 copper Substances 0.000 title claims abstract description 179
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 121
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 121
- 239000002131 composite material Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000843 powder Substances 0.000 claims abstract description 72
- 238000003825 pressing Methods 0.000 claims abstract description 45
- 239000001301 oxygen Substances 0.000 claims abstract description 40
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 40
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 38
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 36
- 150000001875 compounds Chemical class 0.000 claims abstract description 33
- 238000001125 extrusion Methods 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000006185 dispersion Substances 0.000 claims abstract description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 13
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 13
- 239000005749 Copper compound Substances 0.000 claims abstract description 9
- 238000000889 atomisation Methods 0.000 claims abstract description 9
- 150000001880 copper compounds Chemical class 0.000 claims abstract description 9
- 238000001514 detection method Methods 0.000 claims abstract description 3
- 238000007689 inspection Methods 0.000 claims abstract description 3
- 229910045601 alloy Inorganic materials 0.000 claims description 46
- 239000000956 alloy Substances 0.000 claims description 46
- 229910017767 Cu—Al Inorganic materials 0.000 claims description 38
- 238000002844 melting Methods 0.000 claims description 19
- 230000008018 melting Effects 0.000 claims description 19
- 239000001257 hydrogen Substances 0.000 claims description 17
- 229910052739 hydrogen Inorganic materials 0.000 claims description 17
- 239000007800 oxidant agent Substances 0.000 claims description 14
- 230000001590 oxidative effect Effects 0.000 claims description 14
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 13
- 238000005245 sintering Methods 0.000 claims description 13
- 229910017888 Cu—P Inorganic materials 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 8
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 8
- 229940112669 cuprous oxide Drugs 0.000 claims description 8
- 150000002431 hydrogen Chemical class 0.000 claims description 8
- 238000007254 oxidation reaction Methods 0.000 claims description 7
- 230000003647 oxidation Effects 0.000 claims description 6
- 230000010354 integration Effects 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000003610 charcoal Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000007499 fusion processing Methods 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000011812 mixed powder Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000004663 powder metallurgy Methods 0.000 abstract description 4
- 238000005219 brazing Methods 0.000 description 6
- 239000002245 particle Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 241001124569 Lycaenidae Species 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000000181 anti-adherent effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 235000014987 copper Nutrition 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- -1 ferrous metals Chemical class 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
- B21C37/04—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of bars or wire
-
- B22F1/0003—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
- B22F3/04—Compacting only by applying fluid pressure, e.g. by cold isostatic pressing [CIP]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Powder Metallurgy (AREA)
Abstract
A kind of preparation method of dispersion-strengthened Cu and oxygen-free copper composite bar, preparation flow step are as follows: nitrogen atomization powder → prepared by oxygen source → mixes powder → isostatic cool pressing processing → short route, integrated heat treatment → extrusion process → finishing, decortication → dispersion-strengthened Cu and the compound copper ingot preparation → dispersion-strengthened Cu of oxygen-free copper and the compound copper ingot secondary extrusion → dispersion-strengthened Cu of oxygen-free copper and oxygen-free copper compound bar stretch process → inspection and detection；Pass through powder metallurgy and pressure processing technology, the nano dispersion reinforced copper of Cu-Al2O3 and oxygen-free copper are carried out compound, it is prepared into the nano dispersion reinforced copper of Cu-Al2O3 and oxygen-free copper composite bar, using the characteristic of the advanced oxygen-free copper of elevated temperature strength of the nano dispersion reinforced copper of Cu-Al2O3, to meet the needs of electronics and information industry platinotron and electric utility large-current high-voltage relay etc. are to critical material.
Description
Technical field
The present invention relates to have powder metallurgy and non-ferrous metals processing field more particularly to a kind of dispersion-strengthened Cu and oxygen-free copper
The preparation method of composite bar.
Background technique
Dispersion-strengtherning is by introducing stable, uniform, tiny oxide particle, pinning dislocation, crystalline substance in metallic matrix
Boundary, sub boundary hinder the movement of dislocation, thus the method for strengthening material；Dispersion-strengthened Cu is due to the Dispersed precipitate in Copper substrate
The oxide particle of fine uniform, intensity is higher, and softening temperature is high；Simultaneously small and dispersed distribution oxide particle again not
Adverse effect can be caused to the electrical and thermal conductivity of copper alloy itself, so that dispersion-strengthened Cu is also able to maintain while improving intensity
Itself excellent electrical and thermal conductivity；Therefore, dispersion-strengthened Cu be comprehensive electric conductivity, thermal conductivity, room temperature and elevated temperature strength, hardness and
Wearability, resistance fusion welding can highest copper alloys.
Currently, dispersion-strengthened Cu is in industrial circles such as microwave device, automobile, battery, Electronic Packaging, high-voltage relays
In be widely used；The industrial process of dispersion strengthening copper alloy is internal oxidation, and main points are using oxidant
Cu-Al alloy powder is aoxidized, also original acquisition high-strength highly-conductive Cu-Al2O3 resistant to high temperature then is carried out to oxide powder
Nano dispersion reinforced copper alloy；This method preparation dispersion strengthening copper alloy reinforced phase be it is generated in-situ, with matrix have it is excellent
Different associativity, internal oxidition can make reinforced phase even particle distribution, and size is tiny；
Dispersion-strengthened Cu is that good hot strong, height leads material, is well suited for doing inner chamber body and high current in platinotron
High-voltage relay contact material, but its brazing property is poor, is typical anti-adhesive material, with the materials such as oxygen-free copper, stainless steel
Welding effect it is bad, weld seam is not able to satisfy the requirement of the materials such as the microwave tube outer chamber of high-air-tightness requirement；
Oxygenless copper material has excellent electrical and thermal conductivity performance, microwave device and new-energy automobile large-current high-voltage after
Electrical contact, vacuum high-voltage switch etc. are well used；But in the preparation process of microwave tube and high-voltage relay,
It needs to carry out high temperature brazing with materials such as other oxygen-free coppers, stainless steel, ceramics in hydrogen atmosphere, temperature is 800 DEG C~930
DEG C, it welds at this temperature, the softening of oxygenless copper material is very serious；Oxygenless copper material is able to satisfy common microwave tube and high pressure
The use of relay, but platinotron and large-current high-voltage relay purposes contact material, oxygen-free copper are then difficult to win
Appoint；
Dispersion copper and oxygen-free copper are combined, being made into outer layer is oxygen-free copper, and internal layer is the composite bar of dispersion copper, can sufficiently be sent out
The excellent brazing property of the softening performance and oxygen-free copper resistant to high temperatures of dispersion copper is waved, the composite bar that the two performance advantage is combined,
It is well positioned to meet the devices application such as outer chamber and large-current high-voltage relay in platinotron, meets industry requirement；
With electronics and information industry and the development of electric utility, market is to platinotron and large-current high-voltage relay
Demand it is increasing, the market prospects of dispersion-strengthened Cu and oxygen-free copper composite bar are very good；
Currently, domestic tens patents in relation to dispersion copper, the technology of preparing of related dispersion-strengthened Cu mostly use greatly short stream
Journey technology of preparing, but dispersion-strengthened Cu and oxygen-free copper is not found to carry out the compound technology for being prepared into composite bar；How to lead to
Powder metallurgy and pressure processing technology are crossed, the nano dispersion reinforced copper of Cu-Al2O3 and oxygen-free copper progress is compound, it is prepared into Cu-
The nano dispersion reinforced copper of Al2O3 and oxygen-free copper composite bar promote the comprehensive performance of dispersion-strengthened Cu and oxygen-free copper composite bar,
As insoluble technical problem for a long time.
In view of the foregoing, the preparation method of a kind of dispersion-strengthened Cu and oxygen-free copper composite bar is now developed.
Summary of the invention
Purpose of the invention is to overcome the shortcomings in the prior art, provides a kind of dispersion-strengthened Cu and oxygen-free copper is compound
The preparation method of bar, by powder metallurgy and pressure processing technology, the nano dispersion reinforced copper of Cu-Al2O3 and oxygen-free copper into
Row is compound, is prepared into the nano dispersion reinforced copper of Cu-Al2O3 and oxygen-free copper composite bar, nano dispersion reinforced using Cu-Al2O3
The characteristic of the advanced oxygen-free copper of the elevated temperature strength of copper is high to meet electronics and information industry platinotron and electric utility high current
The demand to critical material such as potential relay.
The present invention to achieve the goals above, adopts the following technical scheme that a kind of dispersion-strengthened Cu and oxygen-free copper compound bar
The preparation method of material, nitrogen atomization powder → prepared by oxygen source → mix powder → isostatic cool pressing processing → short route, integration heat treatment
→ extrusion process → finishing, decortication → dispersion-strengthened Cu and the compound copper ingot preparation → dispersion-strengthened Cu of oxygen-free copper and oxygen-free copper are compound
Copper ingot secondary extrusion → dispersion-strengthened Cu and oxygen-free copper compound bar stretch process → inspection and detection；
Nitrogen atomization powder: the first step carries out melting using 100kg mid-frequency melting furnace, adds first in mid-frequency melting furnace
Enter high-purity the melting of anaerobic electrolytic copper 40~70 minutes, fusion process is covered with charcoal；Then 0.5~3 point of Cu-P alloy deoxidation is added
Clock, the ratio that the ratio of Cu is P in 86~88%, Cu-P alloy in Cu-P alloy is 11~15%, adds Cu-Al conjunction
Golden melting 3~8 minutes, the ratio of Cu is the ratio 28~32% of Al in 69~71%, Cu-Al alloy, Al in Cu-Al alloy
Content in Cu-Al alloy is controlled in 0.05~0.9wt%, then carries out atomization system with the nitrogen of 0.7~1.0Mpa pressure
Powder, drying screen out -100 mesh Cu-Al alloy starting powders；
Oxygen source preparation: second step -100 mesh Cu-Al alloy starting powders is sieved again, screen out -200 mesh Cu -
Al powder aoxidizes 20~80 hours at 200 DEG C~500 DEG C, and then under the conditions of nitrogen protection, 600 DEG C~900 DEG C resolve into oxidation
Cuprous solid oxygen source；
Third step mixes powder: the cuprous oxide solid oxygen source and -100 original powder of mesh Cu-Al alloy of -200 mesh obtained
Last formula according to the ratio calculates the additive amount of the cuprous oxide solid oxygen source of -200 mesh, the ratio formula: M/N=9A/8B
× P, M are the original powder weight of Cu-Al alloy, and N is oxidant weight, and A is the weight percent of aluminium in the original powder of Cu-Al alloy
The weight percent of oxidant oxygen content, hydrogen loss value can replace, and B is the weight percent of oxidant oxygen content, and P is oxidant
Coefficient of excess 0.3~0.9, mixing time are 0.5~1.5 hour；
Isostatic cool pressing processing: 4th step the disperse copper alloy powder mixed in proportion is carried out with isostatic cool pressing gum cover
Sealing, shakes 1~3 minute on bobbing machine, keeps apparent density uniform, green density is consistent, is then sealed with rubber cap, then use
Iron wire fastening；The gum cover of packaged disperse copper alloy powder is put into progress isostatic cool pressing processing in isostatic cool pressing cylinder body and is made cold etc.
Static pressure powder ingot, pressing pressure: 180~300Mpa, the rate of rise: 10~20Mpa/ minutes, the dwell time 5~10 minutes；
Short route, integration heat treatment: 5th step is put into isostatic cool pressing powder ingot in heat-treatment furnace flue, according to interior oxygen
Change, reduction, the integrated heat treatment of sequence progress being sintered；
Internal oxidition processing is that the Al in isostatic cool pressing powder ingot is allowed to be converted into Al2O3, internal oxidition temperature: 850 DEG C~950 DEG C, interior
Oxidization time: 2~6 hours, protective atmosphere: nitrogen；
Reduction temperature: 880 DEG C~980 DEG C, the recovery time: 2~6 hours, reducing atmosphere: high-purity hydrogen, dew point: -60 DEG C,
Oxygen content: ≯ 10PPm；
Sintering temperature: 900 DEG C~960 DEG C, sintering time: 2~6 hours, sintering atmosphere: high-purity hydrogen, dew point: -60 DEG C,
Oxygen content: ≯ 10PPm；
Extrusion process: isostatic cool pressing powder ingot after heat treatment is carried out sheathed extrusion or directly naked ingot squeezes, In by the 6th step
It is squeezed, isostatic cool pressing powder ingot heating temperature: 850 DEG C~960 DEG C, heating time: 2~4 hours, being squeezed on 4000 tons of extruders
Pressure ratio 7~35, squeezing bar gauge lattice is 75~Φ of Φ 85mm；
7th step, finishing, decortication: it is after extruding extrude stick gone end to end, align, remove sheet copper, be worked into Φ 70
~Φ 80mm；
Prepared by the 8th step, dispersion-strengthened Cu and the compound copper ingot of oxygen-free copper: extruding stick oil removing, cleaning, encapsulation what is processed
To 100/ 77.5 × 300mm of Φ of Φ, with a thickness of in the heavy wall anaerobic copper sheathing of 10~15mm, anaerobic copper sheathing both ends are welded with no-oxygen copper plate
Sealing is connect, 100/ 77.5 × 300mm of Φ dispersion-strengthened Cu of Φ and the compound copper ingot of oxygen-free copper are prepared into；
9th step, dispersion-strengthened Cu and the compound copper ingot secondary extrusion of oxygen-free copper: 100/ Φ 77.5 of Φ prepared ×
300mm dispersion-strengthened Cu and the compound copper ingot of oxygen-free copper carry out secondary extrusion, and extruding specification is 20~Φ of Φ 30mm, and composite ingot squeezes
Pressing temperature is 850 DEG C~960 DEG C, heating time: 2~4 hours, extrusion ratio 12~35；
Tenth step, dispersion-strengthened Cu and oxygen-free copper compound bar stretch process: dispersion copper and nothing after secondary extrusion is processed
Oxygen copper is compound extrude stick aligned, go end to end, stretch process to 10~Φ of Φ 30mm；
11st step is checked and is detected: checking outer layer oxygen-free copper thickness are as follows: 1.5~4.5mm detects material property: conductive
Rate: 80%IACS~94%IACS；900 DEG C, Rm:345Mpa~540Mpa, Rp0.2:257Mpa after hydrogen treat half an hour
~430Mpa.
The beneficial effects of the present invention are: the present invention is that the excellent high temperature resistance of dispersion-strengthened Cu and oxygen-free copper is good
Brazing property organically combines, formed have complementary advantages, the two it is compound, greatly improve the comprehensive performance of material, be made disperse
Strengthen copper and oxygen-free copper compound bar have high intensity, high conductivity, softening power resistant to high temperatures by force and with oxygen-free copper, nickel, ceramics
The good feature of the brazing property of material, after 900 DEG C of heat treatments, yield strength is 8~15 times of oxygen-free copper, and conductivity is up to 78
~95%IACS.The compound bar is able to satisfy microwave device and new-energy automobile large-current high-voltage D.C. contactor to the resistance to height of material
Temperature and good brazing property need.
Detailed description of the invention
The present invention will be further explained below with reference to the attached drawings:
Fig. 1 is process flow chart.
Specific embodiment
Below with reference to embodiment, invention is further described in detail with specific embodiment:
Embodiment 1
A kind of dispersion-strengthened Cu for microwave tube outer chamber and oxygen-free copper composite bar；
Nitrogen atomization powder: the first step carries out melting using 100kg mid-frequency melting furnace, adds first in mid-frequency melting furnace
Enter high-purity the melting of anaerobic electrolytic copper 40~70 minutes, fusion process is covered with charcoal；Then 0.5~3 point of Cu-P alloy deoxidation is added
Clock, the ratio that the ratio of Cu is P in 86~88%, Cu-P alloy in Cu-P alloy is 11~15%, adds Cu-Al conjunction
Golden melting 3~8 minutes, the ratio of Cu is the ratio 28~32% of Al in 69~71%, Cu-Al alloy, Al in Cu-Al alloy
Content in Cu-Al alloy is controlled in 0.09~0.14wt%, is then atomized with the nitrogen of 0.7~1.0Mpa pressure
Powder processed, drying screen out -100 mesh Cu-Al alloy starting powders；
Oxygen source preparation: second step -100 mesh Cu-Al alloy starting powders is sieved again, screen out -200 mesh Cu -
Al powder aoxidizes 20~80 hours at 200 DEG C~500 DEG C, and then under the conditions of nitrogen protection, 600 DEG C~900 DEG C resolve into oxidation
Cuprous solid oxygen source；
Third step mixes powder: the cuprous oxide solid oxygen source and -100 original powder of mesh Cu-Al alloy of -200 mesh obtained
Last formula according to the ratio calculates the additive amount of the cuprous oxide solid oxygen source of -200 mesh, the ratio formula: M/N=9A/8B
× P, M are the original powder weight of Cu-Al alloy, and N is oxidant weight, and A is the weight percent of oxidant oxygen content, hydrogen loss value
It can replace, B is the weight percent of aluminium in the original powder of Cu-Al alloy, and P is oxidant coefficient of excess 0.3~0.9, when mixing
Between be 0.5~1.5 hour；
4th step, isostatic cool pressing processing: by 263/ Φ 251 of disperse copper alloy powder Φ mixed in proportion ×
520mm isostatic cool pressing gum cover is sealed, and is shaken 1~3 minute on bobbing machine, is kept apparent density uniform, and green density is consistent,
Then it is sealed with rubber cap, then is fastened with iron wire；The gum cover of packaged disperse copper alloy powder be put into isostatic cool pressing cylinder body into
Isostatic cool pressing powder ingot is made in the processing of row isostatic cool pressing, pressing pressure: 220Mpa, the rate of rise: 10Mpa/ minutes, the dwell time 8
Minute；The size of isostatic cool pressing powder ingot is 232 × 385mm of Φ；
Short route, integration heat treatment: 5th step is put into isostatic cool pressing powder ingot in heat-treatment furnace flue, according to interior oxygen
Change, reduction, the integrated heat treatment of sequence progress being sintered；
Internal oxidition processing is that the Al in isostatic cool pressing powder ingot is allowed to be converted into Al2O3, internal oxidition temperature: 880 DEG C, when internal oxidition
Between: 2 hours, protective atmosphere: nitrogen；
Reduction temperature: 900 DEG C, the recovery time: 3 hours, reducing atmosphere: high-purity hydrogen, dew point: -60 DEG C, oxygen content:
5PPm；
Sintering temperature: 930 DEG C, sintering time: 3 hours, sintering atmosphere: high-purity hydrogen, dew point: -60 DEG C, oxygen content:
5PPm；
Extrusion process: isostatic cool pressing powder ingot after heat treatment is carried out sheathed extrusion or directly naked ingot squeezes, In by the 6th step
Squeezed on 4000 tons of extruders, isostatic cool pressing powder ingot heating temperature: 900 DEG C, heating time: 3 hours, extrusion ratio 20 was squeezed
Bar gauge lattice are Φ 80mm；
7th step, finishing, decortication: it is after extruding extrude stick gone end to end, align, remove sheet copper, be worked into Φ
77mm；
Prepared by the 8th step, dispersion-strengthened Cu and the compound copper ingot of oxygen-free copper: extruding stick oil removing, cleaning, encapsulation what is processed
To 100/ 77.5 × 300mm of Φ of Φ, with a thickness of in the heavy wall anaerobic copper sheathing of 10~15mm, anaerobic copper sheathing both ends are welded with no-oxygen copper plate
Sealing is connect, 100/ 77.5 × 300mm of Φ dispersion-strengthened Cu of Φ and the compound copper ingot of oxygen-free copper are prepared into；
9th step, dispersion-strengthened Cu and the compound copper ingot secondary extrusion of oxygen-free copper: 100/ Φ 77.5 of Φ prepared ×
300mm dispersion-strengthened Cu and the compound copper ingot of oxygen-free copper carry out secondary extrusion, and extruding specification is Φ 24mm, the extruding temperature of composite ingot
It is 900 DEG C, heating time: 3 hours, extrusion ratio 19；
Tenth step, dispersion-strengthened Cu and oxygen-free copper compound bar stretch process: dispersion copper and nothing after secondary extrusion is processed
Oxygen copper is compound extrude stick aligned, go end to end, stretch process to Φ 20mm；
11st step is checked and is detected: checking outer layer oxygen-free copper thickness are as follows: 1.5~4.5mm detects material property: conductive
Rate: 92%IACS；900 DEG C, Rm:350Mpa, Rp0.2:262Mpa after hydrogen treat half an hour.
Embodiment 2
A kind of large-current high-voltage relay contact dispersion-strengthened Cu of new-energy automobile and oxygen-free copper composite bar；
Nitrogen atomization powder: the first step carries out melting using 100kg mid-frequency melting furnace, adds first in mid-frequency melting furnace
Enter high-purity the melting of anaerobic electrolytic copper 40~70 minutes, fusion process is covered with charcoal；Then 0.5~3 point of Cu-P alloy deoxidation is added
Clock, the ratio that the ratio of Cu is P in 86~88%, Cu-P alloy in Cu-P alloy is 11~15%, adds Cu-Al conjunction
Golden melting 3~8 minutes, the ratio of Cu is the ratio 28~32% of Al in 69~71%, Cu-Al alloy, Al in Cu-Al alloy
Content in Cu-Al alloy is controlled in 0.56~0.67wt%, is then atomized with the nitrogen of 0.7~1.0Mpa pressure
Powder processed, drying screen out -100 mesh Cu-Al alloy starting powders；
Oxygen source preparation: second step -100 mesh Cu-Al alloy starting powders is sieved again, screen out -200 mesh Cu -
Al powder aoxidizes 20~80 hours at 200 DEG C~500 DEG C, and then under the conditions of nitrogen protection, 600 DEG C~900 DEG C resolve into oxidation
Cuprous solid oxygen source；
Third step mixes powder: the cuprous oxide solid oxygen source and -100 original powder of mesh Cu-Al alloy of -200 mesh obtained
Last formula according to the ratio calculates the additive amount of the cuprous oxide solid oxygen source of -200 mesh, the ratio formula: M/N=9A/8B
× P, M are the original powder weight of Cu-Al alloy, and N is oxidant weight, and A is the weight percent of oxidant oxygen content, hydrogen loss value
It can replace, B is the weight percent of aluminium in the original powder of Cu-Al alloy, and P is oxidant coefficient of excess 0.3~0.9, when mixing
Between be 0.5~1.5 hour；
4th step, isostatic cool pressing processing: by 263/ Φ 251 of disperse copper alloy powder Φ mixed in proportion ×
520mm isostatic cool pressing gum cover is sealed, and is shaken 1~3 minute on bobbing machine, is kept apparent density uniform, and green density is consistent,
Then it is sealed with rubber cap, then is fastened with iron wire；The gum cover of packaged disperse copper alloy powder be put into isostatic cool pressing cylinder body into
Isostatic cool pressing powder ingot is made in the processing of row isostatic cool pressing, pressing pressure: 220Mpa, the rate of rise: 10Mpa/ minutes, the dwell time 10
Minute；The size of isostatic cool pressing powder ingot is 232 × 385mm of Φ；
Short route, integration heat treatment: 5th step is put into isostatic cool pressing powder ingot in heat-treatment furnace flue, according to interior oxygen
Change, reduction, the integrated heat treatment of sequence progress being sintered；
Internal oxidition processing is that the Al in isostatic cool pressing powder ingot is allowed to be converted into Al2O3, internal oxidition temperature: 930 DEG C, when internal oxidition
Between: 2 hours, protective atmosphere: nitrogen；
Reduction temperature: 920 DEG C, the recovery time: 3 hours, reducing atmosphere: high-purity hydrogen, dew point: -60 DEG C, oxygen content:
5PPm；
Sintering temperature: 950 DEG C, sintering time: 3 hours, sintering atmosphere: high-purity hydrogen, dew point: -60 DEG C, oxygen content:
5PPm；
Extrusion process: isostatic cool pressing powder ingot after heat treatment is carried out sheathed extrusion or directly naked ingot squeezes, In by the 6th step
Squeezed on 4000 tons of extruders, isostatic cool pressing powder ingot heating temperature: 900 DEG C, heating time: 3 hours, extrusion ratio 20 was squeezed
Bar gauge lattice are Φ 80mm；
7th step, finishing, decortication: it is after extruding extrude stick gone end to end, align, remove sheet copper, be worked into Φ
77mm；
Prepared by the 8th step, dispersion-strengthened Cu and the compound copper ingot of oxygen-free copper: extruding stick oil removing, cleaning, encapsulation what is processed
To 100/ 77.5 × 300mm of Φ of Φ, with a thickness of in the heavy wall anaerobic copper sheathing of 10~15mm, anaerobic copper sheathing both ends are welded with no-oxygen copper plate
Sealing is connect, 100/ 77.5 × 300mm of Φ dispersion-strengthened Cu of Φ and the compound copper ingot of oxygen-free copper are prepared into；
9th step, dispersion-strengthened Cu and the compound copper ingot secondary extrusion of oxygen-free copper: 100/ Φ 77.5 of Φ prepared ×
300mm dispersion-strengthened Cu and the compound copper ingot of oxygen-free copper carry out secondary extrusion, and extruding specification is Φ 24mm, the extruding temperature of composite ingot
It is 920 DEG C, heating time: 3 hours, extrusion ratio 19；
Tenth step, dispersion-strengthened Cu and oxygen-free copper compound bar stretch process: dispersion copper and nothing after secondary extrusion is processed
Oxygen copper is compound extrude stick aligned, go end to end, stretch process to Φ 16mm；
11st step is checked and is detected: checking outer layer oxygen-free copper thickness are as follows: 1.5~4.5mm detects material property: conductive
Rate: 81.6%IACS；900 DEG C, Rm:535Mpa, Rp0.2:425Mpa after hydrogen treat half an hour.
Claims (1)
1. the preparation method of a kind of dispersion-strengthened Cu and oxygen-free copper composite bar, it is characterised in that: preparation flow step are as follows: nitrogen
Powder by atomization → prepared by oxygen source → mix powder → isostatic cool pressing processing → short route, integrated heat treatment → extrusion process → finishing,
Decortication → dispersion-strengthened Cu and the compound copper ingot preparation → dispersion-strengthened Cu of oxygen-free copper and the compound copper ingot secondary extrusion of oxygen-free copper → more
It dissipates and strengthens copper and oxygen-free copper compound bar stretch process → inspection and detection；
The first step, nitrogen atomization powder: carrying out melting using 100kg mid-frequency melting furnace, is added first in mid-frequency melting furnace high
Pure the melting of anaerobic electrolytic copper 40~70 minutes, fusion process was covered with charcoal；Then it is added the deoxidation of Cu-P alloy 0.5~3 minute,
The ratio that the ratio of Cu is P in 86~88%, Cu-P alloy in Cu-P alloy is 11~15%, and it is molten to add Cu-Al alloy
It refines 3~8 minutes, the ratio of Cu is the ratio 28~32% of Al in 69~71%, Cu-Al alloy in Cu-Al alloy, and Al exists
Content in Cu-Al alloy is controlled in 0.05~0.9wt%, then carries out atomization system with the nitrogen of 0.7~1.0Mpa pressure
Powder, drying screen out -100 mesh Cu-Al alloy starting powders；
Oxygen source preparation: second step -100 mesh Cu-Al alloy starting powders is sieved again, screen out -200 mesh Cu-Al
Powder aoxidizes 20~80 hours at 200 DEG C~500 DEG C, and then under the conditions of nitrogen protection, 600 DEG C~900 DEG C resolve into oxidation Asia
Copper solid oxygen source；
Mixed powder: third step presses the cuprous oxide solid oxygen source of -200 mesh obtained and -100 mesh Cu-Al alloy starting powders
Ratio formula calculates the additive amount of the cuprous oxide solid oxygen source of -200 mesh, the ratio formula: M/N=9A/8B × P, M
For the original powder weight of Cu-Al alloy, N is oxidant weight, and A is the weight percent oxidation of aluminium in the original powder of Cu-Al alloy
The weight percent of agent oxygen content, hydrogen loss value can replace, and B is the weight percent of oxidant oxygen content, and P is that oxidant is superfluous
Coefficient 0.3~0.9, mixing time are 0.5~1.5 hour；
4th step, isostatic cool pressing processing: the disperse copper alloy powder mixed in proportion is sealed with isostatic cool pressing gum cover,
It is shaken 1~3 minute on bobbing machine, keeps apparent density uniform, green density is consistent, is then sealed with rubber cap, then use iron wire
Fastening；The gum cover of packaged disperse copper alloy powder is put into isostatic cool pressing cylinder body and carries out the obtained isostatic cool pressing of isostatic cool pressing processing
Powder ingot, pressing pressure: 180~300Mpa, the rate of rise: 10~20Mpa/ minutes, the dwell time 5~10 minutes；
5th step, short route, integration heat treatment: being put into isostatic cool pressing powder ingot in heat-treatment furnace flue, according to internal oxidition, also
Former, sintering sequence carries out integrated heat treatment；
Internal oxidition processing is that the Al in isostatic cool pressing powder ingot is allowed to be converted into Al2O3, internal oxidition temperature: 850 DEG C~950 DEG C, internal oxidition
Time: 2~6 hours, protective atmosphere: nitrogen；
Reduction temperature: 880 DEG C~980 DEG C, the recovery time: 2~6 hours, reducing atmosphere: high-purity hydrogen, dew point: -60 DEG C, oxygen contained
Amount: ≯ 10PPm；
Sintering temperature: 900 DEG C~960 DEG C, sintering time: 2~6 hours, sintering atmosphere: high-purity hydrogen, dew point: -60 DEG C, oxygen contained
Amount: ≯ 10PPm；
Extrusion process: isostatic cool pressing powder ingot after heat treatment is carried out sheathed extrusion or directly naked ingot squeezes, 4000 by the 6th step
It is squeezed on ton extruder, isostatic cool pressing powder ingot heating temperature: 850 DEG C~960 DEG C, heating time: 2~4 hours, extrusion ratio
7~35, squeezing bar gauge lattice is 75~Φ of Φ 85mm；
7th step, finishing, decortication: it is after extruding extrude stick gone end to end, align, remove sheet copper, be worked into 70~Φ of Φ
80mm；
Prepared by the 8th step, dispersion-strengthened Cu and the compound copper ingot of oxygen-free copper: extruding stick oil removing, cleaning what is processed, be encapsulated into Φ
100/ 77.5 × 300mm of Φ, with a thickness of in the heavy wall anaerobic copper sheathing of 10~15mm, anaerobic copper sheathing both ends are welded close with no-oxygen copper plate
Envelope, is prepared into 100/ 77.5 × 300mm of Φ dispersion-strengthened Cu of Φ and the compound copper ingot of oxygen-free copper；
9th step, dispersion-strengthened Cu and the compound copper ingot secondary extrusion of oxygen-free copper: more the 100/ 77.5 × 300mm of Φ of Φ prepared
It dissipates and strengthens copper and the compound copper ingot progress secondary extrusion of oxygen-free copper, extruding specification is 20~Φ of Φ 30mm, the extruding temperature of composite ingot
It is 850 DEG C~960 DEG C, heating time: 2~4 hours, extrusion ratio 12~35；
Tenth step, dispersion-strengthened Cu and oxygen-free copper compound bar stretch process: dispersion copper and oxygen-free copper after secondary extrusion is processed
It is compound extrude stick aligned, go end to end, stretch process to 10~Φ of Φ 30mm；
11st step is checked and is detected: checking outer layer oxygen-free copper thickness are as follows: 1.5~4.5mm detects material property: conductivity:
80%IACS~94%IACS；900 DEG C, Rm:345Mpa~540Mpa after hydrogen treat half an hour, Rp0.2:257Mpa~
430Mpa。
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| CN109536771B (en) * | 2018-11-23 | 2020-08-25 | 中铝洛阳铜加工有限公司 | Preparation method of dispersion-strengthened oxygen-free copper alloy plate |
| CN112171031A (en) * | 2020-09-15 | 2021-01-05 | 常州特尔玛枪嘴有限公司 | Conductive nozzle, composite bar thereof and manufacturing process |
| CN112267041B (en) * | 2020-10-26 | 2021-10-15 | 有研工程技术研究院有限公司 | Composite bar and preparation method and application thereof |
| CN112322922B (en) * | 2020-11-14 | 2022-04-22 | 中国兵器科学研究院宁波分院 | Powder metallurgy preparation method of dispersion copper-copper laminated composite material |
| CN112941361B (en) * | 2021-01-25 | 2022-07-12 | 烟台万隆真空冶金股份有限公司 | Dispersion strengthening copper alloy with aluminum oxide distributed in gradient manner and preparation method thereof |
| CN113770365B (en) * | 2021-09-14 | 2023-12-01 | 有研工程技术研究院有限公司 | Dispersion strengthening copper alloy and steel core integrated composite material and preparation method and application thereof |
| CN115319100A (en) * | 2022-08-09 | 2022-11-11 | 中铝洛阳铜加工有限公司 | Preparation process of anti-cracking high-aluminum-content dispersion strengthened copper electrode material |
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