CN102676867B - Alumina particle dispersion strengthened copper composite material and preparation method thereof - Google Patents
Alumina particle dispersion strengthened copper composite material and preparation method thereof Download PDFInfo
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- CN102676867B CN102676867B CN 201210006177 CN201210006177A CN102676867B CN 102676867 B CN102676867 B CN 102676867B CN 201210006177 CN201210006177 CN 201210006177 CN 201210006177 A CN201210006177 A CN 201210006177A CN 102676867 B CN102676867 B CN 102676867B
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Abstract
The invention relates to the technical field of electronic materials, and particularly discloses an alumina particle dispersion strengthened copper composite material and a preparation method thereof. The alumina particle dispersion strengthened copper composite material comprises the following chemical components in percentage by weight: 0.05-1.5 percent of alpha-Al2O3, 0.38-0.94 percent of gamma-Al2O3 and the balance of copper. The preparation method of the alumina particle dispersion strengthened copper composite material provided by the invention has the advantages of short internal oxidation time, low cost and high efficiency. The prepared alumina particle dispersion strengthened copper composite material has high strength, high conductivity, high anti-softening temperature and high high-temperature strength, can meet the requirements of microelectronic industry and electronic information industry on high-conductivity, high-strength and high-temperature-resistant copper alloy andis widely applied to mechanical industry, defense industry and electronic information industry.
Description
Technical field
The present invention relates to technical field of electronic materials, be specifically related to a kind of aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material and preparation method thereof.
Background technology
The electroconductibility of the Cu alloy material of fine copper and the existing trade mark, intensity and high-temperature behavior often are difficult to take into account, and can not satisfy hi-techs such as Aeronautics and Astronautics, microelectronics comprehensively and develop requirement to its over-all properties, Al rapidly
2O
3Dispersion-strengthened Cu (Cu-Al
2O
3) matrix material not only kept copper matrix high conduction, heat conductivility, and have superior high-temperature behavior and etch resistant properties, at aspects such as resistance welding electrode, high strength power line, computer lead frame, conticaster crystallizer, alternative silver based contact material, the tactile bridge of electric switch, welding burners wide application prospect is arranged.
The Glidcop series Cu-Al that U.S. SCM Corporation develops
2O
3Cu-base composites, its softening temperature are 900 ℃, and electric conductivity is 90-92%IACS, and tensile strength also reaches 540MPa, and have formed large-scale production, but its high-temperature behavior, and particularly the high-temperature short delay stretching performance is lower, can not satisfy the requirement of high temperature load-carrying properties.
The manufacturing technology of at present traditional disperse copper adopts powder metallurgic method more, begins to add Al most
2O
3Particle mixes, and carries out sintering after the compression moulding, makes sintered compact.Powder metallurgic method is produced Al
2O
3The dispersion-strengthened Cu technical maturity, the composite property of producing is better, but complex manufacturing, cost height, production efficiency are low, simultaneously the composite material interface vulnerable to pollution.Technology after the improvement is most widely used with oxide powder metallurgy method in the powder, its common technology stream becomes: alloy melting → powder process → interior oxidation → reduction → compacting → sintering → hot-work → cold working, this manufacturing process is by the generated in-situ nano level Al of interior oxidation
2O
3Particle, tiny and be evenly distributed at matrix, higher thermodynamic stability is arranged, but its high-temperature behavior is not good, the flow process complexity causes quality of materials control difficulty simultaneously, and cost is very high, has greatly limited it and has applied.Improve Al
2O
3The high-temperature behavior of dispersion-strengthened carbon/carbon-copper composite material, particularly high temperature tensile properties are the problems that presses for solution at present.
Summary of the invention
The purpose of this invention is to provide a kind of aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material.
Another object of the present invention provides a kind of preparation method of aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material.
In order to realize above purpose, the technical solution adopted in the present invention is: a kind of aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material, its chemical ingredients consists of: weight percentage is α-Al of 0.05～1.5%
2O
3, weight percentage is γ-Al of 0.38～0.94%
2O
3, the copper of surplus.
A kind of preparation method of aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material may further comprise the steps:
(1) batching
Get raw material α-Al
2O
3Powder, Cu
2O and Cu-Al powdered alloy; Prepare burden according to following weight proportion: α-Al
2O
3The weight percentage of powder is 0.05～1.5%, Cu
2The weight percentage of O is 1.90～4.75%, the Cu-Al powdered alloy of surplus; Afterwards raw material is fully mixed;
(2) oxidation in the deformation sintering under vacuum or the protective atmosphere
The raw material that step (1) is prepared places in the graphite jig, put into high temperature sintering furnace then and carry out the sintering oxidation, carry out viscous deformation simultaneously, sintering oven atmosphere is vacuum or rare gas element or decomposed ammonia body, and oxidizing temperature is 950 ℃ in the sintering, and soaking time is 2～4 hours, deformation pressure 30～100MPa, 1～2 hour dwell time made sintered compact, and the diameter of sintered compact is 30～100mm;
(3) hot extrusion
Described sintered compact is heated to 900～1000 ℃, carries out hot extrusion then, extrusion ratio 〉=10, air cooling obtains the hot extrusion bar to room temperature after the hot extrusion;
(4) cold deformation moulding
The hot extrusion bar is carried out cold drawing at the associating cold drawing bench, and the cold drawing deflection is controlled more than 80%, makes aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material.
Preferably, the Cu-Al powdered alloy that described Cu-Al powdered alloy is produced for the water smoke method, the weight percentage of aluminium is 0.20～0.50% in the described Cu-Al powdered alloy, the granularity of described Cu-Al powdered alloy is 37.0～106.0 microns.
Described α-Al
2O
3The granularity of powder is 0.5～5.0 micron, α-Al
2O
3The purity of powder is: α-Al
2O
3Weight percentage 〉=99.5%.
Described Cu
2The granularity of O is 37.0～106.0 microns, described Cu
2The purity of O is: Cu
2The weight percentage of O 〉=99.5%.
Aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material provided by the invention comprises Cu matrix and Al
2O
3Enhanced granule, raw material Cu-Al powdered alloy, α-Al
2O
3Powder and oxygenant Cu
2The O powder is oxidation in the deformation sintering under mixing, vacuum or protective atmosphere, makes the aluminium oxide particles that mixes provided by the invention more and strengthens the dispersion-strengthened carbon/carbon-copper composite material.Raw material α-Al
2O
3The effect of powder mainly is to hinder intercrystalline slip when preventing the high temperature carrying, has the Ao Luowan strengthening effect simultaneously; Oxygenant Cu
2The O effect is pyrolytic decomposition, and active [O] is provided, and with solid solution attitude Al in-situ chemical reaction, raw material nano grade alpha-Al takes place
2O
3Al in particle and the raw material Cu-Al powdered alloy is by Cu
2O oxygenant oxidation original position generates nano level γ-Al
2O
3, the different structure of formation and the Al of different size
2O
3Be evenly distributed on the copper matrix, have dispersion-strengthened effect.
Aluminium oxide particles dispersion-strengthened Cu composite material by adopting provided by the invention mixes Al more
2O
3Technology of preparing makes, and so-called mix, comprises Al more
2O
3Source, structure, size three aspects.Al in aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material provided by the invention
2O
3The source has two, and the one, raw material micron order corundum structure α-Al
2O
3, by pinning copper matrix crystal boundary and obstruction dislocation motion, the high temperature that hinders crystal boundary simultaneously slides to improve the hot strength of aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material; Another is the nano level face-centred cubic structure γ-Al that generates by the Cu-Al alloy inner oxidation
2O
3The pinning subgrain boundary improves the recrystallize drag of deformation matrix, improves the hot mastication drag of aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material, simultaneously since the aluminium atom of solid solution in copper crystal lattice with γ-Al
2O
3Form separate out, so the electroconductibility of copper matrix significantly improves.
The aluminium oxide particles dispersion-strengthened Cu performance of composites index that adopts preparation method provided by the invention to make is: tensile strength 500-610MPa, electric conductivity 80-90%IACS, 600 ℃ of tensile strength 〉=150MPa in short-term.
It is short that the preparation method of aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material provided by the invention has interior oxidization time, cost is low, the advantage that efficient is high, the aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material that makes has high strength, high conductivity, high anti-softening temperature, high hot strength, can satisfy microelectronic industry and electronic information industry and height be led the requirement of high-strength high temperature resistant copper alloy, can be used for resistance welding electrode, the high strength power line, the computer lead frame, conticaster crystallizer, substitute silver based contact material, electric switch touches bridge, fields such as welding burner are in mechanical industry, national defense industry and electronics and information industry have widespread use.
Embodiment
Embodiment 1
The chemical ingredients of the aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material that present embodiment provides consists of: weight percentage is α-Al of 0.05%
2O
3, weight percentage is γ-Al of 0.38%
2O
3, the copper of surplus.
The preparation method of the aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material that present embodiment provides may further comprise the steps:
(1) batching
Get following raw material: the Cu-Al alloy powder that the water smoke method is produced, its aluminium content is 0.20wt%, granularity 37.0-106.0 micron; α-Al
2O
3Powder, granularity 0.5-5.0 micron, purity 〉=99.5wt%; Oxygenant Cu
2The O powder, granularity 37.0-106.0 micron, purity 〉=99.5wt%;
Prepare burden according to following weight proportion: α-Al
2O
3The weight percentage of powder is 0.05%, Cu
2The weight percentage of O is 1.90%, the Cu-Al powdered alloy of surplus;
Adopting V-type to mix the powder machine afterwards fully mixed raw material 3 hours;
(2) oxidation in the vacuum deformation sintering
The raw material powder that step (1) is mixed places in the graphite jig, put into the vacuum high-temperature sintering stove then and carry out the sintering oxidation, carry out viscous deformation simultaneously, oxidizing temperature is 950 ℃ in the sintering, soaking time 4 hours, deformation pressure 35MPa, 1 hour dwell time, this stage is finished the interior oxidation of solid solution Al and the densification of powder mixes body synchronously, makes sintered compact, and the sintered compact diameter is 50mm;
(3) hot extrusion
Described sintered compact is heated to 1000 ℃, carries out hot extrusion at pressing machine, extrusion ratio is 10, obtains the bar of diameter 15.8mm, and air cooling is to room temperature afterwards;
(4) cold deformation moulding
The hot extrusion bar of diameter 15.8mm is carried out the multi-pass cold drawing at 10 tons of associating cold drawing bench of LLB type, and cold drawing to diameter is 7.0mm, and the cold drawing deflection is 80%, makes aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material.
The aluminium oxide particles dispersion-strengthened Cu performance of composites index that the present invention makes is: tensile strength 550MPa, electric conductivity 89%IACS, 600 ℃ of tensile strength 170MPa in short-term.
Embodiment 2
The chemical ingredients of the aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material that present embodiment provides consists of: weight percentage is α-Al of 0.75%
2O
3, weight percentage is γ-Al of 0.66%
2O
3, the copper of surplus.
The preparation method of the aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material that present embodiment provides may further comprise the steps:
(1) batching
Get following raw material: the Cu-Al alloy powder that the water smoke method is produced, its aluminium content is 0.35wt%, granularity 37.0-106.0 micron; α-Al
2O
3Powder, granularity 0.5-5.0 micron, purity 〉=99.5wt%; Oxygenant Cu
2The O powder, granularity 37.0-106.0 micron, purity 〉=99.5wt%;
Prepare burden according to following weight proportion: α-Al
2O
3The weight percentage of powder is 0.75%, Cu
2The weight percentage of O is 3.30%, the Cu-Al powdered alloy of surplus;
Adopting V-type to mix the powder machine afterwards fully mixed raw material 3 hours;
(2) oxidation in the nitrogen protection deformation sintering
The raw material powder that step (1) is mixed places in the graphite jig, put into the atmosphere protection high temperature sintering oven then and carry out the sintering oxidation, carry out viscous deformation simultaneously, protective atmosphere is nitrogen, and oxidizing temperature is 950 ℃ in the sintering, soaking time 2 hours, deformation pressure 60MPa, 2 hours dwell times, this stage is finished the interior oxidation of solid solution Al and the densification of powder mixes body synchronously, make sintered compact, the sintered compact diameter is 80mm;
(3) hot extrusion
Described sintered compact is heated to 950 ℃, carries out hot extrusion at pressing machine, extrusion ratio is 14, obtains the bar of diameter 21.4mm, and air cooling is to room temperature afterwards;
(4) cold deformation moulding
The hot extrusion bar of diameter 21.4mm is carried out the multi-pass cold drawing at 10 tons of associating cold drawing bench of LLB type, and cold drawing to diameter is 9.3mm, and the cold drawing deflection is 81%, makes aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material.
The aluminium oxide particles dispersion-strengthened Cu performance of composites index that the present invention makes is: tensile strength 590MPa, electric conductivity 82%IACS, 600 ℃ of tensile strength 190MPa in short-term.
Embodiment 3
The chemical ingredients of the aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material that present embodiment provides consists of: weight percentage is α-Al of 1.5%
2O
3, weight percentage is γ-Al of 0.94%
2O
3, the copper of surplus.
The preparation method of the aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material that present embodiment provides may further comprise the steps:
(1) batching
Get following raw material: the Cu-Al alloy powder that the water smoke method is produced, its aluminium content is 0.50wt%, granularity 37.0-106.0 micron; α-Al
2O
3Powder, granularity 0.5-5.0 micron, purity 〉=99.5wt%; Oxygenant Cu
2The O powder, granularity 37.0-106.0 micron, purity 〉=99.5wt%;
Prepare burden according to following weight proportion: α-Al
2O
3The weight percentage of powder is 1.5%, Cu
2The weight percentage of O is 4.75%, the Cu-Al powdered alloy of surplus;
Adopting V-type to mix the powder machine afterwards fully mixed raw material 3 hours;
(2) oxidation in the nitrogen protection deformation sintering
The raw material powder that step (1) is mixed places in the graphite jig, put into the atmosphere protection high temperature sintering oven then and carry out the sintering oxidation, carry out viscous deformation simultaneously, protective atmosphere is decomposed ammonia, and oxidizing temperature is 950 ℃ in the sintering, soaking time 4 hours, deformation pressure 35MPa, 2 hours dwell times, this stage is finished the interior oxidation of solid solution Al and the densification of powder mixes body synchronously, make sintered compact, the sintered compact diameter is 100mm;
(3) hot extrusion
Described sintered compact is heated to 1000 ℃, carries out hot extrusion at pressing machine, extrusion ratio is 18, obtains the bar of diameter 23.6mm, and air cooling is to room temperature afterwards;
(4) cold deformation moulding
The hot extrusion bar of diameter 23.6mm is carried out the multi-pass cold drawing at 10 tons of associating cold drawing bench of LLB type, and cold drawing to diameter is 10.0mm, and the cold drawing deflection is 82%, makes aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material.
The aluminium oxide particles dispersion-strengthened Cu performance of composites index that the present invention makes is: tensile strength 610MPa, electric conductivity 80%IACS, 600 ℃ of tensile strength 200MPa in short-term.
Claims (5)
1. an aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material is characterized in that, the chemical ingredients of described aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material consists of: weight percentage is α-Al of 0.05～1.5%
2O
3, weight percentage is γ-Al of 0.38～0.94%
2O
3, the copper of surplus.
2. the preparation method of the described aluminium oxide particles dispersion-strengthened of claim 1 carbon/carbon-copper composite material is characterized in that, may further comprise the steps:
(1) batching
Get raw material α-Al
2O
3Powder, Cu
2O and Cu-Al powdered alloy; Prepare burden according to following weight proportion: α-Al
2O
3The weight percentage of powder is 0.05～1.5%, Cu
2The weight percentage of O is 1.90～4.75%, the Cu-Al powdered alloy of surplus; Afterwards raw material is fully mixed;
(2) oxidation in the deformation sintering under vacuum or the protective atmosphere
The raw material that step (1) is prepared places in the graphite jig, put into high temperature sintering furnace then and carry out the sintering oxidation, carry out viscous deformation simultaneously, sintering oven atmosphere is vacuum or rare gas element or decomposed ammonia body, and oxidizing temperature is 950 ℃ in the sintering, and soaking time is 2～4 hours, deformation pressure 30～100MPa, 1～2 hour dwell time made sintered compact, and the diameter of sintered compact is 30～100mm;
(3) hot extrusion
Described sintered compact is heated to 900～1000 ℃, carries out hot extrusion then, extrusion ratio 〉=10, air cooling obtains the hot extrusion bar to room temperature after the hot extrusion;
(4) cold deformation moulding
The hot extrusion bar is carried out cold drawing at the associating cold drawing bench, and the cold drawing deflection is controlled more than 80%, makes aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material.
3. the preparation method of aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material according to claim 2, it is characterized in that, the Cu-Al powdered alloy that described Cu-Al powdered alloy is produced for the water smoke method, the weight percentage of aluminium is 0.20～0.50% in the described Cu-Al powdered alloy, and the granularity of described Cu-Al powdered alloy is 37.0～106.0 microns.
4. the preparation method of aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material according to claim 2 is characterized in that, described α-Al
2O
3The granularity of powder is 0.5～5.0 micron, α-Al
2O
3The purity of powder is: α-Al
2O
3Weight percentage 〉=99.5%.
5. the preparation method of aluminium oxide particles dispersion-strengthened carbon/carbon-copper composite material according to claim 2 is characterized in that, described Cu
2The granularity of O is 37.0～106.0 microns, described Cu
2The purity of O is: Cu
2The weight percentage of O 〉=99.5%.
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| CN104476843A (en) * | 2014-12-22 | 2015-04-01 | 深圳市锦发铜铝有限公司 | Wear-resistant copper-abased composite board |
| CN104561638B (en) * | 2015-01-04 | 2016-06-08 | 河南科技大学 | A kind of Al2O3The preparation method of dispersed and strengthened copper-based composite material |
| CN110093530A (en) * | 2019-06-10 | 2019-08-06 | 河南科技大学 | It is a kind of high to lead wear-resistant copper based composites and preparation method thereof |
| CN110899717A (en) * | 2019-12-04 | 2020-03-24 | 上海理工大学 | Al (aluminum)2O3-CNTs/Cu composite material and preparation method 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 |
| CN114990373B (en) * | 2022-05-30 | 2023-05-12 | 河南科技大学 | Preparation method of aluminum oxide dispersion strengthening copper-based composite material |
| CN115502606B (en) * | 2022-10-13 | 2023-09-01 | 江西铜业技术研究院有限公司 | Cu/alpha-Al for resistance welding 2 O 3 Preparation method of gradient composite electrode |
| CN116043052B (en) * | 2023-01-16 | 2024-09-10 | 中南大学 | Nano dispersion strengthening copper alloy and preparation method and application thereof |
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