CN109825733A - A kind of short flow process of dispersion strengthening copper alloy - Google Patents
A kind of short flow process of dispersion strengthening copper alloy Download PDFInfo
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- CN109825733A CN109825733A CN201910181250.2A CN201910181250A CN109825733A CN 109825733 A CN109825733 A CN 109825733A CN 201910181250 A CN201910181250 A CN 201910181250A CN 109825733 A CN109825733 A CN 109825733A
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Abstract
The present invention provides a kind of short flow processes of dispersion strengthening copper alloy, gas-atomized powder after Cu-Al alloy compositions melting is first obtained Cu-Al alloy powder by this method, then control oxidation Cu-Al alloy powder, after being mixed later with carbon dust, isostatic cool pressing obtains billet, hydrogen reducing processing will be carried out after billet internal oxidition, finally by hot extrusion deformation after annealing after billet jacket.The short flow process of dispersion strengthening copper alloy of the present invention, it will in the prior art, the technique that oxidant is mixed with copper aluminium powder again after being prepared separately, it is changed to make the oxygen source of internal oxidition of the Cu-Al alloy powder of direct oxidation, simultaneously by internal oxidition and hydrogen reduction process integration, process flow is shortened, labor intensity is reduced.
Description
Technical field
The invention belongs to powder metallurgical technologies, and in particular to a kind of short route preparation side of dispersion strengthening copper alloy
Method.
Background technique
Dispersion strengthening copper alloy is a kind of new structure functional material with excellent combination physical property and mechanical property,
It has both high strength & high electric-conduction can be with good softening performance resistant to high temperatures.The common preparation method packet of dispersion strengthening copper alloy
It includes: mechanical mixing, coprecipitation, nitrate fusion method and internal oxidation etc..Dispersion-strengthened Cu is prepared using internal oxidation to close
Gold is maximally efficient method.
In the prior art, internal oxidation is prepared there are two types of the techniques of dispersion strengthening copper alloy.The first: copper-aluminum alloy powder
Preparation-oxidant preparation-copper aluminium powder mixes with oxidant-and internal oxidition-is broken-reduction-isostatic cool pressing-cold change of jacket-pressurization-
Shape；Second: copper-aluminum alloy powder preparation-oxidant preparation-copper aluminium powder is mixed with oxidant-isostatic cool pressing-internal oxidition/also
Original-jacket-pressurization-cold deformation.As CN101240387B discloses a kind of Cu-Al2O3Nano strengthened dispersion alloy and its preparation side
Method, step include the vacuum melting of Cu-Al alloy, atomization, screening, internal oxidition, hydrogen reducing, vacuum hotpressing, Canned Hot etc.
Process.CN105506329B discloses a kind of high Al2O3Concentration C u-Al2O3The preparation method of nano strengthened dispersion alloy, the party
Method includes: the preparation of Cu-Al alloy powder, mixing, an internal oxidition, high-energy mechanical ball milling, secondary internal oxidition, hydrogen reducing, two
Secondary mixing, cold moudling, vacuum canning and are hot extruded into bar etc..It is tiny that this method first uses an internal oxidation to generate
Al2O3Dispersed granules, then use mechanical alloying high-energy ball milling internal oxidition powder, then to ball-milled powder use secondary internal oxidition with
Further oxidation remnants Al.
In above two technique, it is dirty to easily lead to alloy powder in the process for the first technology process long flow path, time and effort consuming
Dye, influences the conductivity and intensity of dispersion copper.Second of technique is integrated by internal oxidition and hydrogen reduction process, i.e. copper aluminium powder
It is mixed with oxidant, hydrogen reducing is directly carried out after isostatic cool pressing internal oxidition, although shortening process flow, however, due to interior
The temperature of oxidation is high, and powder can bond during internal oxidition, and when leading to hydrogen reducing, remaining oxygen cannot restore completely
Come, even if containing only the oxygen of 100ppm in the copper of 100g, can also generate 14cm in 800 DEG C of hydrogen annealings3High-pressure steam
And copper is caused to rupture, cracked rear air-tightness drastically reduces.In addition, prior art preparation dispersion strengthening copper alloy is both needed to additionally
Add oxidant.
Therefore, height is led to meet the rapid development in the fields such as aerospace, telecommunications, is heat-resisting, disperse oxygen-free copper
The higher demand that " matter " proposes still needs to a kind of new preparation method.
Summary of the invention
To solve to prepare the problems of dispersion strengthening copper alloy in the prior art, the purpose of the present invention is to provide
A kind of short flow process of dispersion strengthening copper alloy.
To achieve the above object, the invention adopts the following technical scheme:
A kind of short flow process of dispersion strengthening copper alloy, step include:
(1) by Cu-Al alloy powder oxidation weight gain；
(2) after step (1) treated Cu-Al alloy powder and carbon dust mix, isostatic cool pressing obtains billet；
(3) reduction treatment after the billet internal oxidition of step (2) is obtained into finished product.
In dispersion strengthening copper alloy, Al2O3Volumn concentration be 0.23~3.33vol%.
Preferably, the temperature of step (1) described oxidation is 300~400 DEG C.
Preferably, the mass percent of step (1) oxidation process Cu-Al alloy powder weight gain be 0.13~
6.49%.
Preferably, the additive amount of carbon dust is the 0.04~1.94% of Cu-Al alloy powder quality in step (2).
The addition of carbon dust makes the oxygen in the cuprous oxide and copper oxide that surface is formed when the control oxidation of Cu-Al alloy powder,
In the heating process of subsequent internal oxidition, it on the one hand can internally spread and react to form Al with Al2O3Nano particle, simultaneously
It can also react to form CO with carbon2, CO2It can produce certain pressure, so that billet is maintained the gap of connection, be directly changed into
After hydrogen atmosphere, hydrogen reducing can be carried out to internal oxidition billet online, shorten process flow, and in traditional handicraft, need elder generation
Hydrogen reducing could be passed through after internal oxidition powder is crushed.
Preferably, the pressure of isostatic cool pressing described in step (2) is 150~300MPa.
During isostatic cool pressing, controlled as controlling the volume of green compact it is final obtained by billet density, make billet
Density is 70~80%.
Preferably, the temperature of step (3) described internal oxidition is 850~890 DEG C.
Preferably, the time of step (3) described internal oxidition is 5~8h.
Internal oxidition refers to that the billet for obtaining isostatic cool pressing heats in atmosphere of inert gases.
Preferably, the temperature of step (3) described reduction treatment is 860~900 DEG C.
Preferably, the time of step (3) described reduction treatment is 5~8h.
Preferably, the gas of step (3) described reduction treatment is hydrogen.
Wherein, Cu-Al alloy powder can weigh Cu-Al alloy compositions according to the ratio, and gas-atomized powder after melting obtains
Cu-Al alloy powder, the temperature of melting are 1200~1230 DEG C, and the alloy melt obtained after melting uses nitrogen aerosolization system
Powder, nitrogen gas purity >=99.9%.
The oxidation of step (1), which refers to, aoxidizes Cu-Al alloy powder under air conditions, monitors during oxidation
The mass change of Cu-Al alloy powder, when the quality of Cu-Al alloy powder increases to setting value, oxidation process terminates.
After step (3), finished product is annealed after fine copper jacket, hot extrusion, deformation under the conditions of argon gas, hot extrusion
Temperature is 880~920 DEG C, extrusion ratio >=15.Be deformed into cold drawing or it is cold swage, deflection be 40~80%.The heat preservation temperature of annealing
Degree is 500~700 DEG C, and soaking time is 40~80min.
The beneficial effect of technical solution of the present invention
1, compared with prior art, the short flow process of dispersion strengthening copper alloy of the present invention, will in the prior art, oxygen
The technique that agent is mixed with copper aluminium powder again after being prepared separately is changed to do internal oxidition with the Cu-Al alloy powder of direct oxidation
Oxygen source, while by internal oxidition and hydrogen reduction process integration, process flow is shortened, labor intensity is reduced, without additional
Add oxidant；
2, in preparation method of the invention, due to the addition of carbon dust, form surface when the control oxidation of Cu-Al alloy powder
Cuprous oxide and copper oxide in oxygen, in the heating process of subsequent internal oxidition, on the one hand can internally spread and and Al
Reaction forms Al2O3Nano particle, the cuprous oxygen in copper oxide of simultaneous oxidation can also react to form CO with carbon2, CO2It can be with
Certain pressure is generated, billet is made to maintain the gap of connection, it, can be online to internal oxidition billet after being directly changed into hydrogen atmosphere
Hydrogen reducing is carried out, ensure that residual oxygen can be restored thoroughly.
Specific embodiment
The following is specific embodiments of the present invention, and further retouches to technical solution of the present invention work in conjunction with the embodiments
It states, however, the present invention is not limited to these examples.
Embodiment 1
This example provides a kind of short flow process of dispersion strengthening copper alloy, key step includes:
(1) by Cu-Al alloy powder oxidation weight gain；
(2) after step (1) treated Cu-Al alloy powder and carbon dust mix, isostatic cool pressing obtains billet；
(3) reduction treatment after the billet internal oxidition of step (2) is obtained into finished product.
In dispersion strengthening copper alloy, Al2O3Volumn concentration be 0.23~3.33vol%.
Wherein, the temperature of step (1) oxidation is 300~400 DEG C, the quality hundred of oxidation process Cu-Al alloy powder weight gain
Divide than being 0.13~6.49%.
The additive amount of carbon dust is the 0.04~1.94% of Cu-Al alloy powder quality in step (2).The addition of carbon dust, makes
The oxygen in cuprous oxide and copper oxide that surface is formed when the control oxidation of Cu-Al alloy powder, in the heated of subsequent internal oxidition
On the one hand Cheng Zhong can internally spread and react to form Al with Al2O3Nano particle, while can also react to be formed with carbon
CO2, CO2It can produce certain pressure, billet made to maintain the gap of connection, it, can be online after being directly changed into hydrogen atmosphere
Hydrogen reducing is carried out to internal oxidition billet, shortens process flow, and in traditional handicraft, it needs after being first crushed internal oxidition powder
Hydrogen reducing can be passed through.
The pressure of isostatic cool pressing is 150~300MPa in step (2), during isostatic cool pressing, passes through control green compact
Volume controls the density of final gained billet, makes the density 70~80% of billet.
The temperature of step (3) internal oxidition is 850~890 DEG C, and the time of internal oxidition is 5~8h, and internal oxidition refers to will be cold etc.
The billet that static pressure obtains heats in atmosphere of inert gases.
The temperature of step (3) reduction treatment is 860~900 DEG C, and the time of reduction treatment is 5~8h, the gas of reduction treatment
Body is hydrogen.
Cu-Al alloy powder can weigh Cu-Al alloy compositions according to the ratio, and gas-atomized powder after melting obtains Cu-Al conjunction
Bronze end, the temperature of melting are 1200~1230 DEG C, and the alloy melt obtained after melting uses nitrogen gas-atomized powder, and nitrogen is pure
Degree >=99.9%.
The oxidation of step (1), which refers to, aoxidizes Cu-Al alloy powder under air conditions, monitors during oxidation
The mass change of Cu-Al alloy powder, when the quality of Cu-Al alloy powder increases to setting value, oxidation process terminates.
After step (3), finished product is annealed after fine copper jacket, hot extrusion, deformation under the conditions of argon gas, hot extrusion
Temperature is 880~920 DEG C, extrusion ratio >=15.Be deformed into cold drawing or it is cold swage, deflection be 40~80%.The heat preservation temperature of annealing
Degree is 500~700 DEG C, and soaking time is 40~80min.
Embodiment 2
This example is specifically prepared for a kind of dispersion strengthening copper alloy A, specific steps are as follows:
(1) Cu-Al alloy compositions are weighed by the proportion that Al content is 0.05wt%, using high-purity after melting at 1210 DEG C
Nitrogen atomization powder obtains Cu-Al alloy powder；
(2) the Cu-Al alloy powder that control oxidation step (1) obtains, specially by alloy powder in 350 DEG C of progress oxygen
Change, after powder weight weight gain 0.22%, comes out and cools down；
(3) by step (2) control oxidation after Cu-Al alloy powder with 0.06% carbon dust mix after, control density exist
70% isostatic cool pressing, isostatic cool pressing obtain billet；
(4) by after 880 DEG C of internal oxidition 7h of billet of step (3), 900 DEG C of hydrogen reducing 5h, the billet after being restored；
(5) step (4) treated billet is subjected to oxygen-free copper suitcase set, 900 DEG C of hot extrusions, then cold deformation of swaging,
Deflection 60% anneals the bar swaged 1 hour at 600 DEG C.
Embodiment 3
This example is specifically prepared for a kind of dispersion strengthening copper alloy B, specific steps are as follows:
(1) Cu-Al alloy compositions are weighed by the proportion that Al content is 0.6%, uses High Purity Nitrogen after melting at 1220 DEG C
Gas-atomized powder obtains Cu-Al alloy powder；
(2) the Cu-Al alloy powder that control oxidation step (1) obtains, specially by alloy powder in 400 DEG C of progress oxygen
Change, after powder weight weight gain 3.2%, comes out and cools down；
(3) by step (2) control oxidation after Cu-Al alloy powder with 0.87% carbon dust mix after, control density exist
70% isostatic cool pressing, isostatic cool pressing obtain billet；
(4) by after 890 DEG C of internal oxidition 7h of billet of step (3), 900 DEG C of hydrogen reducing 7h, the billet after being restored；
(5) step (4) treated billet is subjected to oxygen-free copper suitcase set, 920 DEG C of hot extrusions, then cold deformation of swaging,
Deflection 60% anneals the bar swaged 1 hour at 600 DEG C.
Embodiment 4
This example is specifically prepared for a kind of dispersion strengthening copper alloy C, specific steps are as follows:
(1) Cu-Al alloy compositions are weighed by the proportion that Al content is 0.12%, uses High Purity Nitrogen after melting at 1220 DEG C
Gas-atomized powder obtains Cu-Al alloy powder；
(2) the Cu-Al alloy powder that control oxidation step (1) obtains, specially by alloy powder in 300 DEG C of progress oxygen
Change, after powder weight weight gain 0.96%, comes out and cools down；
(3) by step (2) control oxidation after Cu-Al alloy powder with 2% carbon dust mix after, control density 70%
Isostatic cool pressing, isostatic cool pressing obtain billet；
(4) by after 890 DEG C of internal oxidition 7h of billet of step (3), 900 DEG C of hydrogen reducing 7h, the billet after being restored；
(5) step (4) treated billet is subjected to oxygen-free copper suitcase set, 910 DEG C of hot extrusions, then cold deformation of swaging,
Deflection 60% anneals the bar swaged 1 hour at 600 DEG C.
Detect example
This example tests the performance of dispersion strengthening copper alloy A, B and C of the preparation of embodiment 2~4, and the results are shown in Table 1.
1 dispersion strengthening copper alloy the performance test results of table
| Alloy number | Conductivity/%IACS | Tensile strength/Mpa | Yield strength/MPa | Elongation/% |
| A | 95.2 | 322 | 251 | 19.3 |
| B | 80.1 | 573 | 527 | 15·7 |
| C | 92.3 | 501 | 479 | 17.2 |
Compared with prior art, the short flow process of technical solution of the present invention dispersion strengthening copper alloy, by existing skill
In art, the technique that oxidant is mixed with copper aluminium powder again after being prepared separately is changed to make of the Cu-Al alloy powder of direct oxidation interior
The oxygen source of oxidation, while by internal oxidition and hydrogen reduction process integration, process flow is shortened, labor intensity is reduced.By
In the addition of carbon dust, make the oxygen in the cuprous oxide and copper oxide that surface is formed when the control oxidation of Cu-Al alloy powder, subsequent
In the heating process of internal oxidition, it on the one hand can internally spread and react to form Al with Al2O3Nano particle, simultaneous oxidation are sub-
Oxygen in copper and copper oxide can also react to form CO with carbon2, CO2It can produce certain pressure, billet made to maintain connection
Gap after being directly changed into hydrogen atmosphere, can carry out hydrogen reducing to internal oxidition billet online, ensure that residual oxygen can be thorough
Bottom reduction.
Claims (9)
1. a kind of short flow process of dispersion strengthening copper alloy, which is characterized in that step includes:
(1) by Cu-Al alloy powder oxidation weight gain；
(2) after step (1) treated Cu-Al alloy powder and carbon dust mix, isostatic cool pressing obtains billet；
(3) reduction treatment after the billet internal oxidition of step (2) is obtained into finished product.
2. the short flow process of dispersion strengthening copper alloy according to claim 1, which is characterized in that step (1) is described
The temperature of oxidation is 300~400 DEG C.
3. the short flow process of dispersion strengthening copper alloy according to claim 1, which is characterized in that step (1) is described
The mass percent of oxidation process Cu-Al alloy powder weight gain is 0.13~6.49%.
4. the short flow process of dispersion strengthening copper alloy according to claim 1, which is characterized in that carbon in step (2)
The additive amount of powder is the 0.04~1.94% of Cu-Al alloy powder quality.
5. the short flow process of dispersion strengthening copper alloy according to claim 1, which is characterized in that institute in step (2)
The pressure for stating isostatic cool pressing is 150~300MPa.
6. the short flow process of dispersion strengthening copper alloy according to claim 1, which is characterized in that step (3) is described
The temperature of internal oxidition is 850~890 DEG C.
7. the short flow process of dispersion strengthening copper alloy according to claim 1, which is characterized in that step (3) is described
The time of internal oxidition is 5~8h.
8. the short flow process of dispersion strengthening copper alloy according to claim 1, which is characterized in that step (3) is described
The temperature of reduction treatment is 860~900 DEG C.
9. the short flow process of dispersion strengthening copper alloy according to claim 1, which is characterized in that step (3) is described
The time of reduction treatment is 5~8h.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6376774A (en) * | 1986-09-18 | 1988-04-07 | Sumitomo Light Metal Ind Ltd | Heat resistant high electrical conductivity copper alloy clad material |
| US6039785A (en) * | 1996-02-21 | 2000-03-21 | Bleistahl Produktions-Gmbh & Co. Kg | Material for the powder-metallurgical production of shaped parts, in particular valve seat rings or valve guides with high resistance to wear |
| CN104259692A (en) * | 2014-10-10 | 2015-01-07 | 中铝洛阳铜业有限公司 | Preparation method for car robot automatic welding station resistance welding electrode |
| CN105483419A (en) * | 2016-01-25 | 2016-04-13 | 江西省科学院应用物理研究所 | Preparation method of high-strength and high-conductivity aluminum oxide dispersion-strengthened copper-based composite |
-
2019
- 2019-03-11 CN CN201910181250.2A patent/CN109825733B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6376774A (en) * | 1986-09-18 | 1988-04-07 | Sumitomo Light Metal Ind Ltd | Heat resistant high electrical conductivity copper alloy clad material |
| US6039785A (en) * | 1996-02-21 | 2000-03-21 | Bleistahl Produktions-Gmbh & Co. Kg | Material for the powder-metallurgical production of shaped parts, in particular valve seat rings or valve guides with high resistance to wear |
| CN104259692A (en) * | 2014-10-10 | 2015-01-07 | 中铝洛阳铜业有限公司 | Preparation method for car robot automatic welding station resistance welding electrode |
| CN105483419A (en) * | 2016-01-25 | 2016-04-13 | 江西省科学院应用物理研究所 | Preparation method of high-strength and high-conductivity aluminum oxide dispersion-strengthened copper-based composite |
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