CN100436634C - Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al2O3 alloy and its production - Google Patents

Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al2O3 alloy and its production Download PDF

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CN100436634C
CN100436634C CNB2005100322082A CN200510032208A CN100436634C CN 100436634 C CN100436634 C CN 100436634C CN B2005100322082 A CNB2005100322082 A CN B2005100322082A CN 200510032208 A CN200510032208 A CN 200510032208A CN 100436634 C CN100436634 C CN 100436634C
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汪明朴
李周
娄花芬
程建奕
郭明星
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Central South University
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Abstract

Zero burning hydrogen swelling nanometer diffusion strengthens Cu-Al2O3 alloy and its preparation method. It includes the smelting of the Cu-Al alloy, atomizing Cu-Al alloy powder by using the high-purity N2, sieving , the preparation of the oxidant, the inner oxidize, the hydrogen restores once, solid reducer B restores again, vacuum heat pressing cementation , hot extrusion and cold forming process. The alloy provides in this invention the alloy compares with no oxygen copper, itssigma0.2 is 3-11times higher than no oxygen copper, the temperature of resisting anneal softening can be above 900DEG C, and the electric conduction rate may amount to 75%IACS-96%IACS, it has the characteristic of zero fever hydrogen swelling, it can be applied to the high-pressure cock electric conduction pole , automobile electric resistance welding electrode, the large-scale integrated circuit fuse frame, conticaster crystallizer , the fabrication of the heat sink component which is controlled by the thermonuclear reaction, it is also suitable to the fabrication of the electricity vacuum air seal documents and high precise documents such as microwave tube , X-ray tube , atomsmasher etc.

Description

Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al 2O 3Alloy And Preparation Method
Technical field
The present invention relates to a kind of Cu-Al 2O 3Alloy And Preparation Method.
Background technology
Fine copper (as C10100, TU1 etc.) though electroconductibility high (98～102%IACS), the too low (σ of intensity 0.250MPa only).Though Cu-Fe-P system, Cu-Ni-Si system, Cu-Cr-Zr are that precipitation strength type copper alloy has high strength, high conduction performance, high temperature resistance annealing softening performance is not high, is higher than 500 ℃ and promptly occurs annealing softening rapidly.Nano dispersion reinforced copper alloy is the copper alloy that a class has high strength, high conduction, high temperature resistance annealing softening characteristic, Cu-Al 2O 3Alloy is its important class.Just because of having these excellent specific properties, Cu-Al 2O 3Alloy has obtained widespread use in fields such as electrovacuum microwave tube, large-scale integrated circuit lead frame, high-voltage switch gear conducting rod, automobile resistance welding electrode, conticaster crystallizer, the heat sink parts of controlled thermonuclear reaction.
Cu-Al 2O 3The production method of alloy mainly contains internal oxidation, and the main points of internal oxidation are that the Cu-Al powdered alloy is placed on oxidation in the oxidizing atmosphere, reasonably control oxygen bias voltage and oxidizing temperature, time, forms the resistant to elevated temperatures Cu-Al of high-strength highly-conductive 2O 3Alloy.Number of C u-Al is disclosed both at home and abroad 2O 3The technology of preparing of alloy, wherein typical patent has: US3026200, US3779714, US3884676, US3779714, US4315777, CN1563447-A etc.The method of these patent disclosures can be summarized as follows: with Cu-Al powdered alloy and Cu 2O (oxygenant) powder is by generating Al 2O 3Required chemistry is than mixing, and packs in the copper container in 850 ℃～950 ℃ insulation 0.5～1h with the isostatic cool pressing powder billet state of pulverulence or 80% density, in the insulating process, utilizes Cu 2O emits oxygen and makes in the Cu-Al powdered alloy and be oxidized to Cu-Al 2O 3Powder is removed Cu-Al through 800 ℃～900 ℃ 1h hydrogen reducings again 2O 3Residual oxygen in powder or the powder billet.The method that patent JP7062467-A proposes is oxide powder and the Al with copper 2O 3Particle powder carries out ball milling to be mixed, and adds deoxidation constituent element C or B in 400 ℃ of reducing atmospheres, goes back the oxide compound of native copper, and die mould, sintering prepare Cu-Al then 2O 3Alloy, patent JP8109422-A have also proposed similar method.In above-mentioned each method, Cu-Al 2O 3Powdered alloy or powder billet are processed into fine and close Cu-Al through subsequent handlings such as hot extrusions 2O 3Alloy material.
In the electrovacuum field; the material that being used for the gas seal member of high vacuum, high-precision confidential paper not only needs to make it has high strength, high conduction performance, and needs this material standing more than 900 ℃ after the high-temperature hydrogen protection soldering dimensional stabilizing and still having high strength and high conduction performance.But in above-mentioned patent, all do not provide Cu-Al 2O 3Whether the alloy macro-size changes this performance behind 900 ℃ of high temperature annealing in hydrogen atmospheres.In fact, aforesaid method is difficult to remain in Cu-Al 2O 3Clean or the emptying of oxygen in the alloy or other gas reductions often causes the alloy high-temp annealing in hydrogen atmosphere to expand, and therefore can not be used for electron tube.
Summary of the invention
Purpose of the present invention just provides a kind of Cu-Al 2O 3Nano dispersion reinforced copper alloy and preparation method thereof, this alloy not only have the performance of high strength, high conduction and high temperature resistance annealing softening, also have zero annealing in hydrogen atmosphere expansible performance especially; Not only can be applicable to the manufacturing of high-voltage switch gear conducting rod, automobile resistance welding electrode, large-scale integrated circuit lead frame, conticaster crystallizer, the heat sink parts of controlled thermonuclear reaction, also be particularly suitable for the manufacturing of electrovacuum gas seal members such as microwave tube, X-x ray tube, particle accelerator and high-precision confidential paper.
Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al 2O 3Alloy, its composition scope is: Al 2O 3: 0.08～1.2wt%, B:0～0.04wt%, surplus is Cu.
Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al 2O 3The preparation method of alloy mainly comprises:
(1) Cu-Al alloy melting
With electrolytic copper (purity 99.99%) and Cu-Al master alloy is raw material, electrolytic copper oven dry back is melted in induction furnace, and 1150 ℃～1250 ℃ of temperature of fusion, melt uses the charcoal through roasting to cover, and contains 0.08～1.2wt%Al by final alloy 2O 3Ratio add the Cu-Al master alloy, molten even back forms the Cu-Al alloy melt of required composition.
(2) high-purity N 2Aerosolization Cu-Al alloy powder
Above-mentioned Cu-Al alloy melt is superheated to 1300 ℃～1350 ℃, pours in the atomisation unit, use greater than 6 * 10 5The Pa high-purity N 2Gas is atomized into the Cu-Al powdered alloy by spraying gun with the Cu-Al alloy melt, for preventing that the Cu-Al alloy should be full of N in advance in the oxidation of droplet state surface in the atomizing in atomizing cup 2Gas, will control during atomizing in the atomizing cup is pressure-fired.Owing to rapid condensation, crystal grain was tiny when atomized powder formed, and crystal boundary can become the rapid passage that oxygen infiltrates when interior oxidation, easily generated thick Al at the crystal boundary place 2O 3Particle.For preventing to generate too much thick Al on the crystal boundary 2O 3Particle, atomized powder can carry out the argon shield annealing that 900 ℃～950 ℃, time are 0.5～1.5h, make Cu-Al powdered alloy grain growth, reduce crystal boundary.
(3) screening, oxygenant preparation
With the fragmentation of annealed Cu-Al powdered alloy, screening, the powder of 70～140 μ m granularities is made the internally oxidized alloy powder and is used.Thin alloy powder below 10 microns is oxidized to CuO through 200～300 ℃ of air heating, again at N 2In 800 ℃～900 ℃ heating 1～2h, CuO is resolved into the bigger Cu of decomposition pressure in the gas atmosphere 2O uses in order to the oxygenant during oxidation in doing.In the preparation process of above-mentioned oxygenant, the Al in the Cu-Al alloy powder of preparation oxygenant is by the interior Al that is oxidized to 2O 3Enhanced particles, so oxygenant composition reality is Cu+Cu 2O+Al 2O 3
(4) interior oxidation
Cu-Al powdered alloy and oxygenant n=8C by formula with screening 1M/9C 2The ratio batching of calculating, m-Cu-Al alloy powder quality in the formula, n-oxygenant quality, C 1Al mass content in the-Cu-Al alloy powder, C 2Oxygen mass content in one oxygenant.Fully carry out for oxidation in guaranteeing, oxygenant can be suitably excessive during batching.The material for preparing is behind abundant batch mixing, in the encloses container of packing into (copper jar), and at N 2In interior oxidized still, be heated to 850 ℃～950 ℃ interior oxidations of carrying out 0.5～1h under the condition of protection, form Cu-Al 2O 3Alloy powder.
(5) hydrogen once reduces
With Cu-Al after the interior oxidation 2O 3Alloy powder fragmentation, screening are put into the belt hydrogen reducing furnace and are once reduced, and reductive condition is: 800 ℃～900 ℃ of temperature, time 0.5～1.5h; Reductive hydrogen is High Purity Hydrogen, and dew point is below-40 ℃.Reductive purpose is can how will remain in Cu-Al after the interior oxidation to the greatest extent 2O 3CuO in the alloy powder, Cu 2O, CuAlO 2And the solid solution hydrogen reduction is fallen.Cu-Al after the reduction 2O 3Powder again with the amorphous B powder batch mixing of granularity＜1 μ m, amorphous B powder add-on is 200～400ppm, uses for vacuum heating-press sintering.The adding of amorphous B powder is in order to remain in Cu-Al by trace behind a hydrogen reducing 2O 3Oxygen in the powder carries out secondary reduction,
(6) vacuum heating-press sintering
With above-mentioned Cu-Al 2O 3The compound of alloy powder and amorphous B powder is packed in the graphite mo(u)ld of vacuum hotpressing machine, is evacuated to 10 -2～10 -3Pa charges into a little higher than 10 5The high-purity Ar gas of Pa, Ar atmospheric pressure a little higher than 10 in guaranteeing the thermocompressor chamber 5Under the condition of Pa, be warming up to 900～950 ℃, and be incubated 1～2h, allow solid reductant B diffuse into Cu-Al 2O 3Alloy powder carries out secondary reduction to residual oxygen, and in this course, the carbon of graphite mo(u)ld is to Cu-Al 2O 3Residual oxygen in the alloy powder also has the secondary reduction effect.Continue to make temperature to remain on 900～950 ℃, and extract Ar gas in the chamber out, make vacuum tightness return to 10 -2～10 -3Pa, fully eliminating remains in Cu-Al 2O 3Entrap bubble in the powder (comprising Ar gas) is then to Cu-Al 2O 3Alloy powder carries out hot pressed sintering, and pressure is greater than 27MPa during hot pressing.After vacuum hotpressing, Cu-Al 2O 3Alloy billet density can reach more than 98%.
(7) hot extrusion and cold shaping processing
Because hot pressing billet density up to more than 98%, therefore can directly be heated to 850～950 ℃, and be hot extruded into bar, tubing or slab material under reducing atmosphere (hydrogen furnace or gas furnace) protective condition.For making Cu-Al 2O 3Alloy high compactionization and make Cu-Al 2O 3Produce the metallurgyization combination between alloy powder particle, the extrusion ratio during hot extrusion should be greater than 16: 1.Rod, pipe, slab through hot extrusion can be through follow-up cold machine-shapings, as cold drawing, cold rolling, cold bar, the tubing of swaging into, the cold rolling sheet material etc. of making.If need annealing, annealing then must be carried out being higher than under 600 ℃ of conditions, and reducing atmosphere (as hydrogen) protection is arranged in the cold working process.
The advantage of alloy provided by the invention is as follows: (as C10100, TU1) compares with oxygen free copper, and alloy of the present invention has the performance advantage of high strength, high temperature resistance annealing softening, its σ 0.2Higher 3～11 times than oxygen free copper, anti-annealing softening temperature can be up to more than 900 ℃, and electric conductivity can reach 96%IACS, high density Cu-Al 2O 3The alloy conductive rate can reach 75%IACS, still belongs to high conduction scope.With Cu-Fe-P system, Cu-Ni-Si system, Cu-Cr-Zr be precipitation strength type alloy phase ratio, under the suitable situation of intensity, Cu-Al 2O 3It is obviously high that alloy conductive is wanted, and have much higher high temperature resistance annealing softening performance.Alloy of the present invention also has zero annealing in hydrogen atmosphere expansion characteristics especially, not only can be applicable to the manufacturing of high-voltage switch gear conducting rod, automobile resistance welding electrode, large-scale integrated circuit lead frame, conticaster crystallizer, the heat sink parts of controlled thermonuclear reaction, also be particularly suitable for the manufacturing of electrovacuum gas seal members such as microwave tube, X-x ray tube, particle accelerator and high-precision confidential paper.
Description of drawings
Fig. 1: process flow diagram of the present invention;
Fig. 2: the contrast of alloy outward appearance, wherein (a): annealing in hydrogen atmosphere cracking Cu-Al 2O 3Alloy, (b) annealing in hydrogen atmosphere foaming Cu-Al 2O 3Alloy, (c) alloy of the present invention;
Fig. 3: alloy metallographic structure photograph and electromicroscopic photograph compare, (a): have annealing in hydrogen atmosphere expansible Cu-Al 2O 3Alloy, (b) alloy of the present invention, (c) alloy TEM photo of the present invention.
Embodiment
Embodiment 1: alloy ingredient is Al 2O 3-0.22wt%, B-300ppm, all the other are Cu.Make the hot pressing billet of Φ 100 by method (1)～(6) described in " invention detailed content "; under the hydrogen shield condition, be heated to 930 ℃ of bars (extrusion ratio 25: 1) that are hot extruded into Φ 20 again; and cold drawing is to the bar (deflection 50%) of Φ 14; cold drawn bar is annealed through the hydrogen shield of 900 ℃ of 1h again; it is as shown in table 1 to record the alloy property data; as seen be under the condition of μ m in measuring accuracy, alloy is not observed the annealing in hydrogen atmosphere swelling.Sample appearance pattern behind the metallographic structure of present embodiment alloy, TEM tissue and the annealing in hydrogen atmosphere is seen Fig. 3 (b), (c) and Fig. 2 (c).As seen the present embodiment alloy is the complete metallurgicalization state of full densification, the distributing Al of 5～20nm of the inner disperse of alloy 2O 3Particle, the particle holdfast dislocation.
Table 1 present embodiment Cu-0.22wt%Al 2O 3The alloy property data
Figure C20051003220800081
Embodiment 2: alloy ingredient is Al 2O 3-0.22wt%, all the other are Cu.Compare with embodiment 1, only do not add secondary reduction agent B, all the other preparation working methods are identical with embodiment 1, and experiment condition is also identical.The alloy property data that record are as shown in table 2, even as seen do not add secondary reduction agent B, press when hot because the C in the graphite mo(u)ld still has the secondary reduction effect in vacuum, vacuum can be removed the gas in the powdered alloy in addition, and alloy also produces annealing in hydrogen atmosphere expansion (the overall dimension increase that records is 3 μ m only) hardly.
Table 2 present embodiment Cu-0.22wt%Al 2O 3The alloy property data
Figure C20051003220800082
Embodiment 3: alloy ingredient is Al 2O 3-0.22wt%, all the other are Cu and inevitable impurity.The same with embodiment 2, do not add secondary reduction agent B yet.Removing hot pressing is to be a bit larger tham 10 5Outside carrying out in the high-purity Ar gas shiled of Pa, all the other preparation methods are identical with embodiment 2, and experiment condition is also identical.The alloy property data that record are as shown in table 3, and as seen hot pressing in high-purity Ar gas can make Cu-Al 2O 3Gassiness in the alloy produces slight annealing in hydrogen atmosphere expansion (about 8～15 μ m).
Table 3 present embodiment Cu-0.22wt%Al 2O 3The alloy property data
Figure C20051003220800083
Embodiment 4: alloy ingredient is Al 2O 3-0.22wt%, all the other are Cu and inevitable impurity.The same with embodiment 2, do not add secondary reduction agent B yet.Alloy prepares back (economizing except adding the B operation) by method (1)～(5) described in " invention detailed content " in the method that (5) are described; being pressed into density through isostatic cool pressing is 80% powder billet; (jar made from no-oxygen copper plate) seals behind jacket; in the protection of reducing atmosphere stove, be heated to 930 ℃; hot extrude becomes excellent base (Φ 100 is squeezed into Φ 25), and cold drawing becomes the bar of Φ 14.The performance of the various state alloys that record is as shown in table 4, and as seen the alloy without vacuum hotpressing has produced tangible annealing in hydrogen atmosphere expansion (30～80 μ m).
Table 4 present embodiment Cu-0.22wt%A
Figure C20051003220800091
Embodiment 5: alloy ingredient is Al 2O 3-1.15wt%, B-300ppm, all the other are copper and inevitable impurity.Make the hot pressing billet of Φ 60 by method (1)～(6) described in " invention detailed content ", be heated to 960 ℃ of bars that are hot extruded into Φ 12 in the hydrogen shield condition again.The extruded bars performance data that records is as shown in table 5, and as seen this alloy strength is very high, and electric conductivity still can reach 80%IACS, and does not have the annealing in hydrogen atmosphere swelling.
Table 5 present embodiment Cu-0.22wt%Al 2O 3The alloy property data

Claims (2)

1. Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al 2O 3Alloy is characterized in that: the composition scope is: Al 2O 3: 0.08～1.2wt%, B:0～0.04wt%, surplus is Cu.
2. Zero-sintering and hydrogen-expansion nano-diffusion reinforced Cu-Al 2O 3The preparation method of alloy, its feature mainly comprises:
(1) Cu-Al alloy melting
Electrolytic copper oven dry back is melted in induction furnace, 1150 ℃～1250 ℃ of temperature of fusion, melt uses the charcoal through roasting to cover, and contains 0.08～1.2wt%Al by final alloy 2O 3Ratio add the Cu-Al master alloy, molten even back forms the Cu-Al alloy melt;
(2) high-purity N 2Aerosolization Cu-Al alloy powder
Above-mentioned Cu-Al alloy melt is superheated to 1300 ℃～1350 ℃, pours in the atomisation unit, use greater than 6 * 10 5The Pa high-purity N 2Gas is atomized into the Cu-Al powdered alloy by spraying gun with the Cu-Al alloy melt, and the argon shield annealing that it is 0.5～1.5h that atomized powder carries out 900 ℃～950 ℃, time makes grain growth;
(3) screening, oxygenant preparation
With the fragmentation of annealed Cu-Al powdered alloy, screening, the powder of 70～140 μ m granularities is made the internally oxidized alloy powder and is used, and the thin alloy powder below 10 microns is oxidized to CuO through 200～300 ℃ of air heating, again at N 2Form Cu in 800 ℃～900 ℃ heating 1～2h in the gas atmosphere 2O;
(4) interior oxidation
Cu-Al internally oxidized alloy powder and oxygenant Cu with screening 2O is n=8C by formula 1M/9C 2The ratio batching of calculating, m-Cu-Al alloy powder quality in the formula, n-oxygenant quality, C 1Al mass content in the-Cu-Al alloy powder, C 2Oxygen mass content in the-oxygenant is prepared burden behind abundant batch mixing, in the encloses container of packing into, and at N 2In interior oxidized still, be heated to 850 ℃～950 ℃ interior oxidations of carrying out 0.5～1h under the condition of protection, form Cu-Al 2O 3Alloy powder;
(5) hydrogen once reduces
With Cu-Al after the interior oxidation 2O 3Alloy powder fragmentation, screening are put into the belt hydrogen reducing furnace and are once reduced, and reductive condition is: 800 ℃～900 ℃ of temperature, time 0.5～1.5h; Cu-Al after the reduction 2O 3Powder again with the amorphous B powder batch mixing of granularity＜1 μ m, amorphous B powder add-on is 200～400ppm;
(6) vacuum heating-press sintering
With above-mentioned Cu-Al 2O 3The compound of alloy powder and amorphous B powder is packed in the graphite mo(u)ld of vacuum hotpressing machine, is evacuated to 10 earlier -2～10 -3Pa charges into 10 again 5The Ar gas of Pa is warming up to 900～950 ℃, and is incubated 1～2h and carries out solid reductant B secondary reduction; Extract Ar gas in the chamber out, make vacuum tightness return to 10 -2～10 -3Pa carries out hot pressed sintering then, forms density greater than 98% hot pressing billet, and hot pressing pressure is greater than 27Mpa;
(7) hot extrusion and cold shaping processing
Under the protection of reducing atmosphere condition, the hot pressing billet is heated to 850～950 ℃, is hot extruded into bar, tubing or slab material; Extrusion ratio during hot extrusion should be greater than 16: 1, through the rod of hot extrusion, pipe, slab through follow-up cold machine-shaping.
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