CN107557609B - A kind of copper alloy and preparation method thereof of single phase nano alumina particle dispersion-strengtherning - Google Patents
A kind of copper alloy and preparation method thereof of single phase nano alumina particle dispersion-strengtherning Download PDFInfo
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Abstract
The invention belongs to powder metallurgy pink collar domains, and in particular to a kind of copper alloy and preparation method thereof of single phase nano alumina particle dispersion-strengtherning.Al in oxidant of the invention2O3Content is 0.2~2.4wt% (mass percent), γ-Al2O3Content: >=95%, γ-Al2O3Average grain diameter D is less than 30nm.Alloy is prepared using the Cu-Al alloyed powder of water atomization or nitrogen atomization as raw material, by processes such as liquid phase reactor synthesis, hydrogen desiccation, compacting, densification, finishing, obtains the single-phase nano alumina particles dispersion strengthening copper alloy of excellent combination property.The present invention is to combine liquid phase medium oxygen supply and in-situ reactive synthesis phase, novel " adaptivity " the liquid phase original reactive synthesis technique of one kind developed.Compared with the existing technology there are the advantages such as short production procedure, simple process, material property stabilization, for widening the material in the application and development in high-end technology field, preparation process and its theory significance for improving dispersion strengthening copper alloy are great.
Description
Technical field
The invention belongs to copper alloy powder metallurgy pink collar domain, it is related to a kind of single phase nano alumina particle dispersion-strengtherning
Copper alloy and preparation method thereof.
Technical background
Dispersion strengthening copper alloy be fusing point is high, hardness is big, the ceramic particle of good thermal stability and chemical stability is equal
A kind of Cu alloy material for being distributed in even disperse in Copper substrate and being formed.It is compared to other schedule of reinforcements, dispersion-strengtherning
Reinforcing particle do not dissolve and grow up at high temperature, there is strong inhibition to dislocation motion and crystal boundary migration, show
The intensity for improving material that lands and softening properties resistant to high temperatures, while the influence that particle scatters free electron is smaller,
Therefore the conductivity of Copper substrate will not be substantially reduced.Dispersion strengthening copper alloy is very widely used, is related to electronics, machinery, system
It makes, nearly all field such as engineer application, aerospace, is particularly applicable to all kinds of resistance welding electrodes, high current welding cable,
Large-scale integrated circuit lead frame, platinotron structural material, various heat exchange materials, mold materials, conticaster knot
Brilliant device liner and structural wood materials and parts, the vertical target cooling fin of divertor, nuclear fusion in the tockmark device of thermonuclear reactor
The antenna mirror design of power electric generator and its cooling tube, ITER application, rocket chamber and rocket nozzle, all kinds of particles
Accelerator, electromagnetic launch system, pulse magnetic field conductive material, electric car, the numerous areas such as bullet train.
The performance of strengthened dispersion alloy depends on the intrinsic property of selected disperse phase.It is used as in Copper substrate more
The type of dephasing has very much, specifically includes that (1) various oxides: Al2O3、ThO2、BeO、ZrO2、CrO2Deng;(2) various boronations
Object, carbide, nitride, silicide: BN, TiB2, TiC, TaC, WC, TiN, AlN, SiC etc.;(3) intermetallic compound:
Fe3Al、Ni3Al etc..The type for reasonably selecting disperse phase can play the strengthening effect of disperse phase to the maximum extent, therefore choosing need to
Follow certain principle: diffusing particle fusing point itself is high, hardness is big, and high temperature flowering structure is stablized, and does not dissolve;In Copper substrate
Solid solubility is small, and diffusion rate is lower;Interface binding power between diffusing particle and matrix is stronger;Diffusing particle is in Copper substrate
Granule size, distribution, volume content, shape, spacing are suitable.Al2O3And Y2O3Property under waiting oxide particles partial size tiny and high temperature
It can stablize, Copper substrate can be added into and be allowed to the Dispersed precipitate in matrix, to prepare oxide dispersion intensifying copper.Wherein
Cu-Al2O3Dispersion strengthening copper alloy is a kind of excellent high-strength, high to lead alloy material.Due to the nanoscale Al of Dispersed precipitate2O3
Particle plays the role of dispersion-strengtherning to Copper substrate, and therefore, which has high intensity, high rigidity, high conductivity and height soft
Change the characteristics such as temperature.Have the characteristics that tissue stabilization, without phase-change, yield strength and tensile strength it is high.Room temperature hardness is high, hardness with
The raising fall of temperature is small, and high-temperature creep resistance is good.Heat, conductivity are high.Processing performance is excellent, and softening temperature is up to
It is 930 DEG C, relatively high in copper alloy, it but is below tungsten copper (1000 DEG C) conductivity, heat dissipation performance is between tungsten copper (220W/m.k)
And between fine copper (390W/m-k).Hardness is more than HRB 84, and intensity is high, and fatigue behaviour and wear-resisting property are good.
Preparation Al at present2O3The main method of dispersion strengthening copper alloy has: internal oxidation, coprecipitation, sol-gel method,
Reaction ball milling method, Mixed volatile oil, reactive spray-deposition method etc..Wherein internal oxidation is current heavy industrialization batch production
High-performance Al2O3The most important means of dispersion strengthening copper alloy, specific preparation process are as follows: Cu-Al (0.1~
1.2wt%) melting → water atomization or nitrogen atomization powder → with oxidant mix → closed container internal oxidition → hydrogen in it is dry
And restore → jacket processing → compacting (hot isostatic pressing or hot pressing etc.) → hot extrusion molding → subsequent finishing → product inspection →
Product packaging.But patent is not to hardening constituent Al both at home and abroad2O3Phase structure controlled.Correlative study shows γ-Al2O3
Compared with α-Al2O3With more excellent performance, crystal structure is easy to the interface that Copper substrate forms coherence or half coherence, is conducive to more
Distribution is dissipated, and reduces the influence to electron scattering.Not yet discovery is to Al at present2O3The relevant report of particle phase composition.
Summary of the invention
The present invention provides a kind of copper alloy and preparation method thereof of single phase nano alumina particle dispersion-strengtherning, particular technique
Scheme is as follows:
A kind of copper alloy of single phase nano alumina particle dispersion-strengtherning has following technical characteristic:
(1) ingredient: Al2O3: 0.2~2.4% (mass percent);
(2) aluminium oxide phase: γ-Al2O3Content: >=95%;
(3) alumina particle: aluminium oxide average grain diameter D is less than 30nm.
For the copper alloy of single phase nano alumina particle dispersion-strengtherning described above, specific preparation method, including with
Lower step:
(1) raw material preparation: water atomization or nitrogen atomization produce the Cu-Al alloyed powder of -80 mesh;
(2) liquid phase reactor synthesizes: Cu-Al alloyed powder, oxidant and abrading-ball being closed in ball grinder, pressed on ball mill
It takes out, is dehydrated after certain technique ball milling;
(3) hydrogen desiccation: liquid phase reactor synthesis composite powder is dried under hydrogen protective atmosphere;
(4) it suppresses: the composite powder after the drying is suppressed on cold isostatic press;
(5) it densifies: the green compact is used into vacuum-sintering+hot extrusion technique, hot pressing+hot extrusion technique or hot isostatic pressing
+ hot extrusion technique carries out densification;
(6) it finishes: the green compact after the densification being finished, various profiles are obtained.
In step (1), the Cu-Al alloy powder raw material is at least one in water atomization or nitrogen atomization Cu-Al alloyed powder
Kind, wherein aluminium content is 0.1~1.2wt%, and granularity requirements are -80 mesh.
In step (2), the oxidant is hydrogen peroxide solution or supersaturated ozone solution, by liquid oxidizer and original
Material Cu-Al alloyed powder is prepared by a certain percentage.
In step (2), the abrading-ball is fine copper ball, and ratio of grinding media to material is 4:1~10:1.
In step (2), the ball mill is agitating ball mill or tumbling ball mill.
In step (2), the ball-milling technology is intermittent ball-milling technology, is shut down 30 minutes after ball milling 2~6 hours, with
Guarantee that the heat generated in mechanical milling process makes powder temperature excessively high, causes the alumina particle of produced in situ excessive;It is shutting down
The oxidant is added in the process, reaction in-situ consistent is allowed to carry out, the alumina particle degree of purity of production is high, size is thin
Small and disperse.Ball-grinding machine band water cooling function effect is best.Accumulating Ball-milling Time is 36~72 hours.
In step (2), the total oxygen-supplying amount of oxidant in ball grinder is added as Al content in Cu-Al alloyed powder in ball grinder
1.1~1.3 times.
In step (2), the dehydrating process is centrifuge dehydration or compressed air filter-press dehydration.
In step (3), the hydrogen desiccation technique is 600~800 DEG C, and soaking time 3~6 hours, hydrogen flowing quantity was
It 20L/ minutes, comes out of the stove after dry, is sieved after broken, obtain the Cu-Al of -80 mesh2O3Composite granule.
In step (4), the isostatic cool pressing technique be 180~240MPa of pressing pressure, the dwell time 5~30 minutes,
Three-level release.
In step (5), the vacuum-sintering densification are as follows: vacuum-sintering, 900~950 DEG C of temperature, heat preservation 2~3
Hour, vacuum degree≤3 × 10-2Pa;
In step (5), the vacuum hotpressing densification are as follows: vacuum heating-press sintering, temperature are 850~950 DEG C, are protected
The warm time 2~3 hours, moulding pressure 40MPa, pressing time was 30 minutes, vacuum degree≤3 × 10-2Pa;
In step (5), the hot isostatic pressing densification are as follows: alloy green compact are subjected to vacuum canning, it is true in jacket
Reciprocal of duty cycle≤3 × 10-2Then Pa is placed in densification in hot isostatic press, specifically comprises the processes of: pressure 100MPa, temperature 850~950
DEG C, heat-insulation pressure keeping time 2 h.
In step (5), the ingot blank after the densification is squeezed into the single-phase of 16~20mm of diameter at 920 DEG C and is received
Rice alumina particle dispersion strengthening copper alloy.
In step (6), by the bar cold drawing of 16~20mm of diameter of hot extrusion to 11~16mm of diameter.
Beneficial effects of the present invention are as follows:
Preparation method of the invention passes through the oxidation of liquid phase using water atomization or the Cu-Al alloy powder raw material of nitrogen atomization
Single-phase γ-Al is produced in mechanical milling process2O3, obtained in conjunction with modern powder metallurgy densification process single-phase nano oxidized
Alumina particles dispersion strengthening copper alloy bar, this method can realize in existing powder metallurgy production line, large-scale production easy to accomplish,
And high production efficiency.
The copper alloy bar of single phase nano alumina particle dispersion-strengtherning in the present invention provides height for welding welding industry
By force, high lead, softening resistant to high temperatures, wear-resisting copper alloy raw material guarantee so that dispersion strengthening copper alloy comprehensive performance has matter
It improves, pushes the development of Domestic Automotive Industry, electronics industry middle and high end components.
Detailed description of the invention
Fig. 1: the copper alloy preparation technology flow chart of single phase nano alumina particle dispersion-strengtherning.
Specific embodiment
The present invention relates to a kind of copper alloys and preparation method thereof of single phase nano alumina particle dispersion-strengtherning, specifically include
Following steps: 1 raw material preparation;The synthesis of 2 liquid phase reactors;3 hydrogen desiccations;4 compactings;5 densifications;6 finishing.
With reference to the accompanying drawing 1 and embodiment it is further illustrated.
Embodiment 1
A kind of copper alloy bar of single phase nano alumina particle dispersion-strengtherning, preparation process the following steps are included:
(1) raw material preparation: the Cu-Al alloyed powder produced using water atomization or nitrogen atomization screens 80 mesh powder below
End is used as raw material, Al content 0.6wt%, and granular size is -80 mesh;
(2) liquid phase reactor synthesizes: taking in step (1) 20 kilograms of raw material powder, is placed in agitating ball mill, is added 40 liters and goes
The fine copper ball of ionized water and 80 kilograms of diameter 6mm, ball-milling technology are intermittent ball-milling technology, are shut down 30 minutes after ball milling 3 hours,
Accumulating Ball-milling Time is 36 hours.H is calculated according to the aluminium content being added in Cu-Al alloyed powder2O2Usage amount, 10 parts of equal part
And divides 10 times and be intermittently added agitating ball mill in shutdown.After use sieve to separate abrading-ball with powder after the completion of ball-milling technology, and
Powder is dehydrated using centrifuge.
(3) hydrogen desiccation: dewatered composite powder is fitted into material boat, is placed in hydrogen furnace, hydrogen desiccation technique is
800 DEG C, 4 hours when heat preservation, hydrogen flowing quantity is 20L/ minute, is cooled to room temperature and comes out of the stove to material, is sieved after broken, acquisition -80
Purpose Cu-Al2O3Composite granule.
(4) it suppresses: by the Cu-Al after the drying2O3Composite granule is packed into gum cover, binds, completely cuts off the dirt of pressure medium
Dye, then be placed in cold isostatic press in suppressed, isostatic cool pressing technique be pressing pressure 200MPa, the dwell time 8 minutes, three
After grade release, green compact is obtained.
(5) it densifies: by the Cu-Al2O3Green compact be placed in vacuum sintering funace in, be evacuated to vacuum degree≤3 ×
10-2Pa, electrified regulation are warming up to 950 DEG C, keep the temperature 3 hours, then start to pressurize, pressure 40MPa pressure maintaining 30 minutes, is then let out
Pressure, cools to room temperature with the furnace, obtains Cu-Al2O3Alloy.Then by Cu-Al at 920 DEG C2O3Alloy extrusion is at diameter 20mm's
Extruded bars.
(6) it finishes: by the finished product bar of the bar cold drawing of the diameter 20mm of hot extrusion to diameter 16mm.
Single phase nano alumina particle dispersion strengthening copper alloy bar manufactured in the present embodiment, main indicator are as follows: Al2O3:
1.3wt%, γ-Al2O3Content: >=96%, γ-Al2O3Average grain diameter D is less than 28nm;Single phase nano alumina particle disperse is strong
Change copper alloy main performance: hardness is greater than 80HRB, and conductivity is greater than 80%IACS, and tensile strength is greater than 580MPa.
Embodiment 2
A kind of copper alloy bar of single phase nano alumina particle dispersion-strengtherning, preparation process the following steps are included:
(1) raw material preparation: the Cu-Al alloyed powder produced using water atomization or nitrogen atomization screens 80 mesh powder below
End is used as raw material, Al content 0.1wt%, and granular size is -80 mesh;
(2) liquid phase reactor synthesizes: taking in step (1) 20 kilograms of raw material powder, is placed in tumbling ball mill, is added 50 liters and goes
The fine copper ball of ionized water and 200 kilograms of diameter 5mm, ball-milling technology are intermittent ball-milling technology, and 30 points are shut down after ball milling 6 hours
Clock, accumulation Ball-milling Time are 72 hours.The use of ozone water solution is calculated according to the aluminium content being added in Cu-Al alloyed powder
Amount, 10 parts of equal part are simultaneously intermittently added agitating ball mill in shutdown points for 10 times.Use after the completion of the ball-milling technology sieve by abrading-ball with
Powder separation, and powder is dehydrated using centrifuge.
(3) hydrogen desiccation: dewatered composite powder is fitted into material boat, is placed in hydrogen furnace, hydrogen desiccation technique is
600 DEG C, 2 hours when heat preservation, hydrogen flowing quantity is 20L/ minute, is cooled to room temperature and comes out of the stove to material, is sieved after broken, acquisition -80
Purpose Cu-Al2O3Composite granule.
(4) it suppresses: by the Cu-Al after the drying2O3Composite granule is packed into gum cover, binds, completely cuts off the dirt of pressure medium
Dye, then be placed in cold isostatic press in suppressed, isostatic cool pressing technique be pressing pressure 180MPa, the dwell time 20 minutes,
After three-level release, green compact is obtained.
(5) it densifies: by the Cu-Al2O3Green compact is placed in vacuum canning, and Vacuum Package, soldering, in vacuum canning
Then the interior vacuum canning for having alloy is placed in hot isostatic pressing furnace, vacuumizes, reach at room temperature by vacuum degree≤3 × 10-2Pa
It is filled with argon gas after 13.332Pa, pressure is made to reach 10MPa, starts to warm up, boosts, to 850 DEG C, pressure 100MPa, heat-insulation pressure keeping 2
Hour, subsequent pressure release cools to room temperature with the furnace, obtains Cu-Al2O3Alloy.Then by Cu-Al at 920 DEG C2O3Alloy extrusion
At the extruded bars of diameter 16mm.
(6) it finishes: by the bar cold drawing of the diameter 16mm of hot extrusion to diameter 13mm or the finished product stick of diameter 11mm
Material.
The copper alloy bar of single phase nano alumina particle dispersion-strengtherning manufactured in the present embodiment, main indicator are as follows:
Al2O3: 0.24wt%, γ-Al2O3Content: >=97%, γ-Al2O3Average grain diameter D is less than 20nm;Single phase nano alumina particle
Dispersion strengthening copper alloy main performance: hardness is greater than 65HRB, and conductivity is greater than 90%IACS, and tensile strength is greater than 476MPa.
Claims (3)
1. a kind of preparation method of the copper alloy of single phase nano alumina particle dispersion-strengtherning, which is characterized in that the copper alloy
Contain Al in ingredient2O3, weight percent content is 0.2~2.4%;Aluminium oxide phase γ-Al2O3, content >=95%;Oxidation
Alumina particles average grain diameter D is less than 30nm;
Specific preparation method the following steps are included:
(1) raw material preparation: -80 mesh Cu-Al alloyed powders that water atomization or nitrogen atomization are produced;
(2) liquid phase reactor synthesizes: Cu-Al alloyed powder, oxidant and abrading-ball being closed in ball grinder, by certain on ball mill
It takes out, is dehydrated after technique ball milling;
The ball-milling technology is intermittent ball-milling technology, and abrading-ball is fine copper ball, and ratio of grinding media to material is 4:1~10:1, and ball milling 2~6 is small
When after shut down 30 minutes, accumulation Ball-milling Time be 36~72 hours;
The oxidant is hydrogen peroxide solution or supersaturated ozone solution, the total oxygen-supplying amount of oxidant being added in ball grinder are
In ball grinder 1.1~1.3 times of Al content in Cu-Al alloyed powder;
(3) hydrogen desiccation: liquid phase reactor synthesis composite powder is dried under protective atmosphere;
The hydrogen desiccation technique is 600~800 DEG C, and soaking time 3~6 hours, hydrogen flowing quantity was 20L/ minutes, after dry
It comes out of the stove, is sieved after broken, obtain the Cu-Al of -80 mesh2O3Composite granule;
(4) it suppresses: the composite powder after the drying is suppressed on cold isostatic press;
(5) it densifies: the green compact is used into vacuum-sintering+hot extrusion technique, hot pressing+hot extrusion technique or hot isostatic pressing+heat
Extrusion process carries out densification;
The hot isostatic pressing densification are as follows: alloy green compact are subjected to vacuum canning, vacuum degree≤3 × 10 in jacket-2Pa,
Then densification in merging hot isostatic press, specifically comprises the processes of: pressure 100MPa, 850~950 DEG C of temperature, the heat-insulation pressure keeping time 2
Hour;
(6) it finishes: the green compact after the densification being finished, various profiles are obtained.
2. a kind of preparation method of the copper alloy of single phase nano alumina particle dispersion-strengtherning according to claim 1,
It is characterized in that, Cu-Al alloy powder raw material described in step (1) is at least one in water atomization or nitrogen atomization Cu-Al alloyed powder
Kind, wherein aluminium content is 0.1~1.2wt%, and granularity requirements are -80 mesh.
3. a kind of preparation method of the copper alloy of single phase nano alumina particle dispersion-strengtherning according to claim 1,
It is characterized in that, dehydrating process described in step (2) is centrifuge dehydration or compressed air filter-press dehydration.
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CN109161824B (en) * | 2018-09-28 | 2020-10-20 | 河南科技大学 | Al (aluminum)2O3TiB-mixed reinforced copper-based composite material, preparation method thereof and preparation method of copper alloy raw material powder |
CN110184489A (en) * | 2019-06-11 | 2019-08-30 | 中山麓科睿材科技有限公司 | A kind of preparation process of alumina dispersion-strenghtened copper alloy |
CN111850377B (en) * | 2020-06-18 | 2022-03-22 | 江苏大学 | In-situ Al2O3Preparation method of particle reinforced aluminum matrix composite |
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 |
CN113122747B (en) * | 2021-04-22 | 2021-11-16 | 合肥工业大学 | Cu- (WC-Y) with excellent mechanical property2O3) Method for preparing composite material |
CN114703391A (en) * | 2022-03-25 | 2022-07-05 | 华中科技大学 | Nano-oxide dispersion strengthened copper alloy and preparation method thereof |
CN114752808A (en) * | 2022-04-19 | 2022-07-15 | 有研工程技术研究院有限公司 | High-strength high-conductivity copper alloy composite material and preparation method thereof |
CN115747553B (en) * | 2022-11-10 | 2023-12-01 | 合肥工业大学 | Method for preparing Cu-based composite material by using deionized water as process control agent and oxidant |
CN115652174B (en) * | 2022-11-11 | 2024-02-02 | 宁波博威合金材料股份有限公司 | Aluminum oxide dispersion strengthening copper alloy and preparation method and application thereof |
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JP4916284B2 (en) * | 2006-11-17 | 2012-04-11 | 住友軽金属工業株式会社 | Method for producing dispersion strengthened alloy |
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