CN108057732A - 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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- CN108057732A CN108057732A CN201711270364.1A CN201711270364A CN108057732A CN 108057732 A CN108057732 A CN 108057732A CN 201711270364 A CN201711270364 A CN 201711270364A CN 108057732 A CN108057732 A CN 108057732A
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- 239000010949 copper Substances 0.000 title claims abstract description 180
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 123
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 123
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 73
- 238000003825 pressing Methods 0.000 claims abstract description 42
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000001301 oxygen Substances 0.000 claims abstract description 38
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 38
- 238000001125 extrusion Methods 0.000 claims abstract description 37
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 34
- 150000001875 compounds Chemical class 0.000 claims abstract description 33
- 238000010438 heat treatment Methods 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 21
- 238000000034 method Methods 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
- 230000008569 process Effects 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
- 238000005245 sintering Methods 0.000 claims description 16
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 13
- 239000007800 oxidant agent Substances 0.000 claims description 13
- 230000001590 oxidative effect Effects 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
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 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
- 230000001681 protective effect Effects 0.000 claims description 8
- 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
- 230000010354 integration Effects 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- 230000009467 reduction Effects 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 7
- 238000004663 powder metallurgy Methods 0.000 abstract description 4
- 238000005219 brazing Methods 0.000 description 6
- 230000008859 change Effects 0.000 description 4
- 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
- 230000008901 benefit Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000002708 enhancing effect 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
- 230000000181 anti-adherent effect Effects 0.000 description 1
- 230000004888 barrier function 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
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 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
- 230000009931 harmful effect 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
-
- 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
Abstract
The preparation method of a kind of dispersion-strengthened Cu and oxygen-free copper composite bar, preparation flow step are：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 technology
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, so as to 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
Harmful effect can be caused to the electrical and thermal conductivity of copper alloy in itself so that dispersion-strengthened Cu can also be kept while intensity is improved
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.
At present, 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 powders are aoxidized, the also heat safe Cu-Al2O3 of original acquisition high-strength highly-conductive is then carried out to oxide powder
Nano dispersion reinforced copper alloy；Dispersion strengthening copper alloy enhancing prepared by this method is mutually generated in-situ, is had with matrix excellent
Different associativity, internal oxidition can make enhancing 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 cannot meet 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 can meet common microwave tube and high pressure
The use of relay, but be then difficult to win for platinotron and large-current high-voltage relay purposes contact material, oxygen-free copper
Appoint；
Dispersion copper and oxygen-free copper are combined, it is oxygen-free copper to make outer layer, and internal layer is the composite bar of dispersion copper, can fully be sent out
The high temperature resistance softening performance of dispersion copper and the brazing property that oxygen-free copper is excellent are waved, the composite bar that the two performance advantage is combined,
The devices application such as outer chamber and large-current high-voltage relay in platinotron is well positioned to meet, 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；
At present, domestic tens patents in relation to dispersion copper, the technology of preparing of related dispersion-strengthened Cu use short stream mostly
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 barrier 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.
The content of the invention
The purpose of the invention is to overcome deficiency of the prior art, it is compound with oxygen-free copper to provide a kind of dispersion-strengthened Cu
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 elevated temperature strength of copper is high to meet electronics and information industry platinotron and electric utility high current
Potential relay etc. is to the demand of critical material.
The present invention to achieve these goals, adopts the following technical scheme that：A kind of dispersion-strengthened Cu and oxygen-free copper compound bar
The preparation method of material, preparation flow step are：Nitrogen atomization powder → prepared by oxygen source → mixes powder → isostatic cool pressing processing → short stream
Journey, integrated heat treatment → extrusion process → finishing, decortication → dispersion-strengthened Cu and the compound copper ingot preparation → disperse of oxygen-free copper are strong
Change 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；
The first step, nitrogen atomization powder：Melting is carried out using 100kg mid-frequency melting furnaces, is added first in mid-frequency melting furnace
Enter high-purity anaerobic electrolytic copper melting 40~70 minutes, fusion process is covered with charcoal；Then 0.5~3 point of Cu-P alloys deoxidation is added in
Clock, the ratio that the ratio of Cu is P in 86~88%, Cu-P alloys in Cu-P alloys is 11~15%, adds Cu-Al conjunctions
Golden melting 3~8 minutes, the ratio of Cu is the ratio 28~32% of Al in 69~71%, Cu-Al alloys in Cu-Al alloys, Al
Content in Cu-Al alloys 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；
It is prepared by second step, oxygen source：- 100 mesh Cu-Al alloys starting powders are sieved again, screen out -200 mesh Cu -
Al powder, when 200 DEG C~500 DEG C oxidations 20~80 are small, then under nitrogen protective condition, 600 DEG C~900 DEG C resolve into oxidation
Cuprous solid oxygen source；
3rd step mixes powder：The cuprous oxide solid oxygen source and -100 original powder of mesh Cu-Al alloys of -200 mesh obtained
End is calculated the additive amount of the cuprous oxide solid oxygen source of -200 mesh, the ratio formula by ratio formula：M/N=9A/8B
× P, M be the original powder weight of Cu-Al alloys, N be oxidant weight, A be oxidant oxygen content weight percent, hydrogen loss value
It can replace, B is the weight percent of aluminium in the original powder of Cu-Al alloys, and P is oxidant coefficient of excess 0.3~0.9, during batch mixing
Between for 0.5~1.5 it is small when；
4th step, isostatic cool pressing processing：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, makes apparent density uniform, green density is consistent, is then sealed with rubber cap, then uses
Iron wire fastens；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, 5~10 minutes dwell times；
5th step, short route, integration heat treatment：Isostatic cool pressing powder ingot is put into heat-treatment furnace flue, according to interior oxygen
Change, reduce, the order of sintering carries out integrated heat treatment；
Internal oxidition processing is that the Al allowed in isostatic cool pressing powder ingot is converted into Al2O3, internal oxidition temperature：850 DEG C~950 DEG C,
The internal oxidition time：2~6 it is small when, protective atmosphere：Nitrogen；
Reduction temperature：880 DEG C~980 DEG C, the recovery time：2~6 it is small when, 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 it is small when, sintering atmosphere：High-purity hydrogen, dew point：- 60 DEG C,
Oxygen content：≯10PPm；
6th step, extrusion process：Isostatic cool pressing powder ingot after heat treatment is carried out sheathed extrusion or directly naked ingot squeezes,
It is squeezed on 4000 tons of extruders, isostatic cool pressing powder ingot heating temperature：850 DEG C~960 DEG C, heating time：2~4 it is small when, squeeze
Pressure ratio 7~35, it is 75~Φ of Φ 85 to squeeze bar gauge lattice；
7th step, finishing, decortication：After extruding extrude stick gone end to end, align, remove sheet copper, be worked into Φ 70
~Φ 80；
8th step, dispersion-strengthened Cu are prepared with the compound copper ingot of oxygen-free copper：Stick oil removing, cleaning, encapsulation are extruded what is processed
To 100/ Φ 77.5 × 300 of Φ, thickness is in the heavy wall anaerobic copper sheathing of 10~15mm, and anaerobic copper sheathing both ends are welded with no-oxygen copper plate
Sealing, is prepared into 100/ Φ of Φ, 77.5 × 300 dispersion-strengthened Cus 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：100/ Φ 77.5 × 300 of Φ prepared
Dispersion-strengthened Cu carries out secondary extrusion with the compound copper ingot of oxygen-free copper, extrudes specification as 20~Φ of Φ 30, the extrusion temperature of composite ingot
For 850 DEG C~960 DEG C, heating time：2~4 it is small when, 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 30；
11st step is checked and detected：Check that outer layer anaerobic copper thickness is：1.5~4.5mm detects material property:It is conductive
Rate：80%IACS~94%IACS；900 DEG C, the Rm after hydrogen treat half an hour：345Mpa~540Mpa, Rp0.2：257Mpa
~430Mpa.
The beneficial effects of the invention are as follows：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, high temperature resistance softening power it is strong and with oxygen-free copper, nickel, ceramics
The characteristics of brazing property of material is good, 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 can meet 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.
Description of the drawings
The invention will be further described below in conjunction with the accompanying drawings：
Fig. 1 is process flow chart.
Specific embodiment
The present invention is described in further detail with specific embodiment with reference to embodiment：
Embodiment 1
A kind of dispersion-strengthened Cu for microwave tube outer chamber and oxygen-free copper composite bar；
The first step, nitrogen atomization powder：Melting is carried out using 100kg mid-frequency melting furnaces, is added first in mid-frequency melting furnace
Enter high-purity anaerobic electrolytic copper melting 40~70 minutes, fusion process is covered with charcoal；Then 0.5~3 point of Cu-P alloys deoxidation is added in
Clock, the ratio that the ratio of Cu is P in 86~88%, Cu-P alloys in Cu-P alloys is 11~15%, adds Cu-Al conjunctions
Golden melting 3~8 minutes, the ratio of Cu is the ratio 28~32% of Al in 69~71%, Cu-Al alloys in Cu-Al alloys, Al
Content in Cu-Al alloys 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；
It is prepared by second step, oxygen source：- 100 mesh Cu-Al alloys starting powders are sieved again, screen out -200 mesh Cu -
Al powder, when 200 DEG C~500 DEG C oxidations 20~80 are small, then under nitrogen protective condition, 600 DEG C~900 DEG C resolve into oxidation
Cuprous solid oxygen source；
3rd step mixes powder：The cuprous oxide solid oxygen source and -100 original powder of mesh Cu-Al alloys of -200 mesh obtained
End is calculated the additive amount of the cuprous oxide solid oxygen source of -200 mesh, the ratio formula by ratio formula：M/N=9A/8B
× P, M be the original powder weight of Cu-Al alloys, N be oxidant weight, A be oxidant oxygen content weight percent, hydrogen loss value
It can replace, B is the weight percent of aluminium in the original powder of Cu-Al alloys, and P is oxidant coefficient of excess 0.3~0.9, during batch mixing
Between for 0.5~1.5 it is small when；
4th step, isostatic cool pressing processing：263/ Φ 251 × 520 of disperse copper alloy powder Φ that will be mixed in proportion
Isostatic cool pressing gum cover is sealed, and is shaken 1~3 minute on bobbing machine, is made apparent density uniform, 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 is put into isostatic cool pressing cylinder body carry out it is cold
Isostatic cool pressing powder ingot, pressing pressure is made in isostatic pressed processing：220Mpa, the rate of rise：10Mpa/ minutes, 8 minutes dwell times；
The size of isostatic cool pressing powder ingot is Φ 232 × 385；
5th step, short route, integration heat treatment：Isostatic cool pressing powder ingot is put into heat-treatment furnace flue, according to interior oxygen
Change, reduce, the order of sintering carries out integrated heat treatment；
Internal oxidition processing is that the Al allowed in isostatic cool pressing powder ingot is converted into Al2O3, internal oxidition temperature：880 DEG C, during internal oxidition
Between：2 it is small when, protective atmosphere：Nitrogen；
Reduction temperature：900 DEG C, the recovery time：3 it is small when, reducing atmosphere：High-purity hydrogen, dew point：- 60 DEG C, oxygen content：
5PPm；
Sintering temperature：930 DEG C, sintering time：3 it is small when, sintering atmosphere：High-purity hydrogen, dew point：- 60 DEG C, oxygen content：
5PPm；
6th step, extrusion process：Isostatic cool pressing powder ingot after heat treatment is carried out sheathed extrusion or directly naked ingot squeezes,
It is squeezed on 4000 tons of extruders, isostatic cool pressing powder ingot heating temperature：900 DEG C, heating time：3 it is small when, extrusion ratio 20, squeeze
Bar gauge lattice are Φ 80；
7th step, finishing, decortication：After extruding extrude stick gone end to end, align, remove sheet copper, be worked into Φ 77；
8th step, dispersion-strengthened Cu are prepared with the compound copper ingot of oxygen-free copper：Stick oil removing, cleaning, encapsulation are extruded what is processed
To 100/ Φ 77.5 × 300 of Φ, thickness is in the heavy wall anaerobic copper sheathing of 10~15mm, and anaerobic copper sheathing both ends are welded with no-oxygen copper plate
Sealing, is prepared into 100/ Φ of Φ, 77.5 × 300 dispersion-strengthened Cus 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：100/ Φ 77.5 × 300 of Φ prepared
Dispersion-strengthened Cu carries out secondary extrusion with the compound copper ingot of oxygen-free copper, extrudes specification as Φ 24, and the extrusion temperature of composite ingot is 900
DEG C, heating time：3 it is small when, 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 20；
11st step is checked and detected：Check that outer layer anaerobic copper thickness is：1.5~4.5mm detects material property:It is conductive
Rate：92%IACS；900 DEG C, the Rm after hydrogen treat half an hour：350Mpa, Rp0.2：262Mpa.
Embodiment 2
A kind of large-current high-voltage relay contact dispersion-strengthened Cu of new-energy automobile and oxygen-free copper composite bar；
The first step, nitrogen atomization powder：Melting is carried out using 100kg mid-frequency melting furnaces, is added first in mid-frequency melting furnace
Enter high-purity anaerobic electrolytic copper melting 40~70 minutes, fusion process is covered with charcoal；Then 0.5~3 point of Cu-P alloys deoxidation is added in
Clock, the ratio that the ratio of Cu is P in 86~88%, Cu-P alloys in Cu-P alloys is 11~15%, adds Cu-Al conjunctions
Golden melting 3~8 minutes, the ratio of Cu is the ratio 28~32% of Al in 69~71%, Cu-Al alloys in Cu-Al alloys, Al
Content in Cu-Al alloys 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；
It is prepared by second step, oxygen source：- 100 mesh Cu-Al alloys starting powders are sieved again, screen out -200 mesh Cu -
Al powder, when 200 DEG C~500 DEG C oxidations 20~80 are small, then under nitrogen protective condition, 600 DEG C~900 DEG C resolve into oxidation
Cuprous solid oxygen source；
3rd step mixes powder：The cuprous oxide solid oxygen source and -100 original powder of mesh Cu-Al alloys of -200 mesh obtained
End is calculated the additive amount of the cuprous oxide solid oxygen source of -200 mesh, the ratio formula by ratio formula：M/N=9A/8B
× P, M be the original powder weight of Cu-Al alloys, N be oxidant weight, A be oxidant oxygen content weight percent, hydrogen loss value
It can replace, B is the weight percent of aluminium in the original powder of Cu-Al alloys, and P is oxidant coefficient of excess 0.3~0.9, during batch mixing
Between for 0.5~1.5 it is small when；
4th step, isostatic cool pressing processing：263/ Φ 251 × 520 of disperse copper alloy powder Φ that will be mixed in proportion
Isostatic cool pressing gum cover is sealed, and is shaken 1~3 minute on bobbing machine, is made apparent density uniform, 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 is put into isostatic cool pressing cylinder body carry out it is cold
Isostatic cool pressing powder ingot, pressing pressure is made in isostatic pressed processing：220Mpa, the rate of rise：10Mpa/ minutes, the dwell time 10 divided
Clock；The size of isostatic cool pressing powder ingot is Φ 232 × 385；
5th step, short route, integration heat treatment：Isostatic cool pressing powder ingot is put into heat-treatment furnace flue, according to interior oxygen
Change, reduce, the order of sintering carries out integrated heat treatment；
Internal oxidition processing is that the Al allowed in isostatic cool pressing powder ingot is converted into Al2O3, internal oxidition temperature：930 DEG C, during internal oxidition
Between：2 it is small when, protective atmosphere：Nitrogen；
Reduction temperature：920 DEG C, the recovery time：3 it is small when, reducing atmosphere：High-purity hydrogen, dew point：- 60 DEG C, oxygen content：
5PPm；
Sintering temperature：950 DEG C, sintering time：3 it is small when, sintering atmosphere：High-purity hydrogen, dew point：- 60 DEG C, oxygen content：
5PPm；
6th step, extrusion process：Isostatic cool pressing powder ingot after heat treatment is carried out sheathed extrusion or directly naked ingot squeezes,
It is squeezed on 4000 tons of extruders, isostatic cool pressing powder ingot heating temperature：900 DEG C, heating time：3 it is small when, extrusion ratio 20, squeeze
Bar gauge lattice are Φ 80；
7th step, finishing, decortication：After extruding extrude stick gone end to end, align, remove sheet copper, be worked into Φ 77；
8th step, dispersion-strengthened Cu are prepared with the compound copper ingot of oxygen-free copper：Stick oil removing, cleaning, encapsulation are extruded what is processed
To 100/ Φ 77.5 × 300 of Φ, thickness is in the heavy wall anaerobic copper sheathing of 10~15mm, and anaerobic copper sheathing both ends are welded with no-oxygen copper plate
Sealing, is prepared into 100/ Φ of Φ, 77.5 × 300 dispersion-strengthened Cus 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：100/ Φ 77.5 × 300 of Φ prepared
Dispersion-strengthened Cu carries out secondary extrusion with the compound copper ingot of oxygen-free copper, extrudes specification as Φ 24, and the extrusion temperature of composite ingot is 920
DEG C, heating time：3 it is small when, 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 16；
11st step is checked and detected：Check that outer layer anaerobic copper thickness is：1.5~4.5mm detects material property:It is conductive
Rate：81.6%IACS；900 DEG C, the Rm after hydrogen treat half an hour：535Mpa, Rp0.2：425Mpa.
Claims (2)
1. a kind of preparation method of dispersion-strengthened Cu and oxygen-free copper composite bar, it is characterised in that：Preparation flow step is：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.
2. the preparation method of a kind of dispersion-strengthened Cu according to claim 1 and oxygen-free copper composite bar, it is characterised in that：
The first step, nitrogen atomization powder：Melting is carried out using 100kg mid-frequency melting furnaces, is added in first in mid-frequency melting furnace high
Pure anaerobic electrolytic copper melting 40~70 minutes, fusion process is covered with charcoal；Then Cu-P alloys deoxidation 0.5~3 minute is added in,
The ratio that the ratio of Cu is P in 86~88%, Cu-P alloys in Cu-P alloys is 11~15%, adds Cu-Al alloys and melts
It refines 3~8 minutes, the ratio of Cu is the ratio 28~32% of Al in 69~71%, Cu-Al alloys in Cu-Al alloys, and Al exists
Content in Cu-Al alloys 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；
It is prepared by second step, oxygen source：- 100 mesh Cu-Al alloys starting powders are sieved again, screen out -200 mesh Cu-Al
Powder, when 200 DEG C~500 DEG C oxidations 20~80 are small, then under nitrogen protective condition, 600 DEG C~900 DEG C resolve into oxidation Asia
Copper solid oxygen source；
3rd step mixes powder：The cuprous oxide solid oxygen source of -200 mesh obtained and -100 mesh Cu-Al alloy starting powders are pressed
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 alloys, N is oxidant weight, and A is the weight percent of oxidant oxygen content, and hydrogen loss value being capable of generation
It replaces, B is the weight percent of aluminium in the original powder of Cu-Al alloys, and P is oxidant coefficient of excess 0.3~0.9, and mixing time is
0.5~1.5 it is small when；
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, makes apparent density uniform, green density is consistent, is then sealed with rubber cap, then uses 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, 5~10 minutes dwell times；
5th step, short route, integration heat treatment：Isostatic cool pressing powder ingot is put into heat-treatment furnace flue, according to internal oxidition, also
Former, sintering order carries out integrated heat treatment；
Internal oxidition processing is that the Al allowed in isostatic cool pressing powder ingot is converted into Al2O3, internal oxidition temperature：850 DEG C~950 DEG C, internal oxidition
Time：2~6 it is small when, protective atmosphere：Nitrogen；
Reduction temperature：880 DEG C~980 DEG C, the recovery time：2~6 it is small when, reducing atmosphere：High-purity hydrogen, dew point：- 60 DEG C, oxygen contains
Amount：≯10PPm；
Sintering temperature：900 DEG C~960 DEG C, sintering time：2~6 it is small when, sintering atmosphere：High-purity hydrogen, dew point：- 60 DEG C, oxygen contains
Amount：≯10PPm；
6th step, extrusion process：Isostatic cool pressing powder ingot after heat treatment is carried out sheathed extrusion or directly naked ingot squeezes, 4000
It is squeezed on ton extruder, isostatic cool pressing powder ingot heating temperature：850 DEG C~960 DEG C, heating time：2~4 it is small when, extrusion ratio
7~35, it is 75~Φ of Φ 85 to squeeze bar gauge lattice；
7th step, finishing, decortication：After extruding extrude stick gone end to end, align, remove sheet copper, be worked into 70~Φ of Φ
80；
8th step, dispersion-strengthened Cu are prepared with the compound copper ingot of oxygen-free copper：Stick oil removing, cleaning are extruded what is processed, is encapsulated into Φ
100/ Φ 77.5 × 300, thickness are in the heavy wall anaerobic copper sheathing of 10~15mm, and anaerobic copper sheathing both ends are welded close with no-oxygen copper plate
Envelope, is prepared into 100/ Φ of Φ, 77.5 × 300 dispersion-strengthened Cus 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：100/ Φ of Φ, 77.5 × 300 disperses prepared
Strengthen copper and carry out secondary extrusion with the compound copper ingot of oxygen-free copper, extrude specification as 20~Φ of Φ 30, the extrusion temperature of composite ingot is 850
DEG C~960 DEG C, heating time：2~4 it is small when, 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 30；
11st step is checked and detected：Check that outer layer anaerobic copper thickness is：1.5~4.5mm detects material property:Conductivity：
80%IACS~94%IACS；900 DEG C, the Rm after hydrogen treat half an hour：345Mpa~540Mpa, Rp0.2：257Mpa~
430Mpa。
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