CN101717872A - Method for preparing nano dispersion reinforced elastic Cu-Nb alloy - Google Patents
Method for preparing nano dispersion reinforced elastic Cu-Nb alloy Download PDFInfo
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- CN101717872A CN101717872A CN200910311922A CN200910311922A CN101717872A CN 101717872 A CN101717872 A CN 101717872A CN 200910311922 A CN200910311922 A CN 200910311922A CN 200910311922 A CN200910311922 A CN 200910311922A CN 101717872 A CN101717872 A CN 101717872A
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Abstract
The invention discloses a method for preparing a nano dispersion reinforced elastic Cu-Nb alloy, comprising the following steps of: preparing low-oxygen Cu-Nb alloy ingot blanks and preparing elastic strips by hot extrusion and cold rolling processes, wherein in the low-oxygen Cu-Nb alloy ingot blank preparation step, the metallurgy ingot blanks are prepared by vacuum or nitrogen protection ball milling, hydrogen protection annealing and vacuum hot pressing on raw material powder; the elastic strip preparation step by hot extrusion and cold rolling processes comprises the hot extrusion and cold rolling deformation, wherein the extrusion ratio is higher than or equal to 15:1 on the metallurgy ingot blanks, the pass deflection is 8-10 percent on extruded material; compared with beryllium bronze, the alloy prepared by the invention has the advantages of higher strength, higher electrical conductivity, better high-temperature annealing and softening property and no poison elements (such as beryllium). The invention has simple process method and convenient operation and can realize batch production. The prepared Cu-Nb alloy has high strength, high electrical conductivity and high anti-stress relaxation ability, thereby being suitable for high-performance current conducting elastic components of aerospace industry and electronic industry, such as high-power hermetically sealed electromagnetic relays and the like.
Description
Technical field
The present invention relates to a kind of preparation method of Cu-Nb alloy, refer in particular to a kind of preparation method of nano dispersion reinforced elastic Cu-Nb alloy; Belong to the mmaterial technical field.This elastic alloy has high strength, high conduction and high resistance to stress relaxation property, can be applicable to space flight and aviation and electronic industry high-performance conductive elastic element, as high-power sealed electromagnetic relay etc.
Background technology
In recent years, industrial expansions such as space flight, aviation, weapons, naval vessel, electronics are had higher requirement to the every technical indicator and the adaptive capacity to environment of resilient material, as as the critical material in the rly., contact spring not only needs electric conductivity height, good springiness, is easy to welding, and requires every stable performance under the hot conditions more than 200 ℃.Though berylliumbronze has high electroconductibility and thermal conductivity, be not suitable for life-time service at high temperature.Though silver-magnesium-nickel alloys conduction, good heat conductivity, anti-electric-arc ability are strong, intensity, Young's modulus are lower, and resilience stability is poor under the high temperature.After novel elastic such as Cu-Ni-Al, the Cu-Ni-Si copper alloy ageing treatment higher elasticity and hardness are arranged, but its stress relaxation resistance can not be competent at the Working environment more than 200 ℃.Cu-Ni-Sn alloy and " Ka Milong " alloy have very high intensity and resilience stability preferably, but its specific conductivity is too low.Nano dispersion reinforced copper alloy is the copper alloy that a class has high strength, high conduction, high temperature resistance annealing softening characteristic, as Cu-Al
2O
3, Cu-Nb alloy etc.Cu-Al wherein
2O
3Though alloy has high high temperature resistance annealing softening ability, because the restriction of interior oxidizing reaction, this alloy system still can not be realized the highly concentrated nano dispersion-strengthened, is not enough to produce sufficiently high elastic performance.The above various materials of introducing are because the defective that its component or weave construction exist causes its over-all properties can not satisfy the requirement of industrial development to every technical indicator of resilient material.
Summary of the invention
The preparation method who the objective of the invention is to overcome the deficiency of prior art and simple, the easy to operate nano dispersion reinforced elastic Cu-Nb alloy of a kind of processing method is provided.Have high strength, high conduction, characteristic that high resistance to stress is lax by the elastic Cu-Nb alloy of the inventive method preparation.
The preparation method of a kind of nano dispersion reinforced elastic Cu-Nb alloy of the present invention may further comprise the steps:
The first step: preparation hypoxemia level Cu-Nb alloy ingot blank
1, press each weight percentages of components of Cu-Nb alloy, get purity 〉=99.95% respectively, mean particle size is Cu powder and purity 〉=99.90% of 10～15 μ m, and the Nb powder of mean particle size＜5 μ m mixes, and is (5～6) * 10 in vacuum tightness
-2Ball milling under Pa or purity＞99.999% high-purity argon gas atmosphere protection, ratio of grinding media to material (15～20): 1, rotational speed of ball-mill 250～350rpm, ball milling time 40～50h makes the strong molten and inner Cu-Nb nanometer crystal alloy powder that contains a large amount of less than 5nm disperse Nb or NbO particle;
2, with Cu-Nb nanometer crystal alloy powder under the hydrogen shield atmosphere in 600～650 ℃ stove, soaking time 1.0～1.5h carries out hydrogen shield annealing; Make CuO, Cu in the Cu-Nb powdered alloy behind the ball milling
2O is reduced to Cu; Then, add the boron powder that accounts for Cu-Nb nanometer crystal alloy powder total amount 50～300ppm in the Cu-Nb nanometer crystal alloy powder after annealing, after mixing, in the vacuum hotpressing machine, carry out hot pressed sintering, make the metallurgical billet of Cu-Nb of oxygen level≤11ppm; The hot-pressing sintering technique parameter is: vacuum tightness 10
-2～10
-3Pa, 800～850 ℃ of temperature, pressure 25～30MPa, hot pressing time 2h; By the online secondary reduction of solid reductant vacuum hotpressing, can further remove the residual oxygen that remains in the alloy;
Second step: hot extrusion and cold-rolling process prepare the elasticity band
1, under the high pure nitrogen protection of purity＞99.999% Cu-Nb powder metallurgy billet is heated to 800～900 ℃, hot extrusion makes the extruding slab; Mould temperature 〉=450 ℃ during hot extrusion, extrusion ratio 〉=15: 1;
2, the extruding slab of gained is carried out pass deformation be 8%～10% cold roller and deformed, when total deformation reaches 34%～35%, cold rolling material is carried out stress relief annealing, 600～750 ℃ of annealing temperatures, soaking time 30～60min under the high pure nitrogen protection of purity＞99.999%; Repeat above-mentioned steps, finally make the cold rolling elasticity band of high precision of thick 0.1～0.5mm.
The present invention adopts above-mentioned processing method, has obtained the strong molten and inner Cu-Nb nanometer crystal alloy powder that contains a large amount of less than 5nm disperse Nb or NbO particle by mechanical ball milling; Because Nb solubleness in copper is extremely low, solid solution Nb separates out more abundant in hot pressing subsequently and hot extrusion process, makes the copper matrix have high purity, thereby has improved alloy conductive greatly; Simultaneously, because the nano dispersion reinforced effect of highly concentrated nano level Nb particle can make the Cu-Nb alloy obtain snappiness; In addition, because the Nb particle has high heat-resistant stability in the Cu-Nb alloy, grow up even under 900 ℃ high temperature, also be difficult to assemble, therefore the Cu-Nb alloy is under 250 ℃ temperature, dislocation configuration extremely difficulty changes, can not produce answer, more not exist born of the same parents' shape to separate out problem, make the Cu-Nb alloy should have higher high temperature stress relaxation-resistant ability.
Alloy of the present invention is compared with berylliumbronze, has intensity height, electric conductivity height, high temperature resistance annealing softening performance is good and does not contain the advantage of poisonous element (as beryllium).QBe
2Use temperature only reaches 150 ℃, and (σ
0-σ
k)/σ
0=25%.The Cu-Nb alloy is through 250 ℃+0.5 σ
0.01Under the prestress condition behind the burin-in process 50h, stress relaxation rate (σ under the 250 ℃/100h condition
0-σ
k)/σ
0≤ 5%.Compare with precipitation strength type elastic alloys such as Cu-Ni-Sn with Cu-Ni-Al, Cu-Ni-Si, under the suitable situation of intensity, Cu-Nb alloy conductive obviously higher (can reach more than the 30%IACS), and do not have intensity, elasticity and electric conductivity that overaging and high temperature Hui Rong the cause problem that sharply descends, anti-annealing softening temperature can be up to more than 900 ℃.
In sum, processing method of the present invention simple, easy to operate, can realize producing in batches; Prepared Cu-Nb alloy has high strength, high conduction, high resistance to stress relaxation property, is applicable to space flight and aviation and electronic industry high-performance conductive elastic element, as high-power sealed electromagnetic relay etc.
Description of drawings
Accompanying drawing 1 (a): be the extruding slab sample photo of the embodiment of the invention 3 preparations.
Accompanying drawing 1 (b): be the cold-strip sample photo of the embodiment of the invention 3 preparations.
Accompanying drawing 2 (a): be the TEM photo of the alloy of the embodiment of the invention 3 preparation.
Accompanying drawing 2 (b): be the electron diffraction pattern of the alloy of the embodiment of the invention 3 preparation.
Being distributed in the Cu matrix of enhanced particles even dispersion from the visible alloy of the present invention of accompanying drawing 2 (a), size is about 5～10nm, and the pinning dislocation makes this alloy have quite high stress relaxation-resistant ability strongly.The electron diffraction pattern of accompanying drawing 2 (b) has proved that enhanced particles is the Nb particle.
Embodiment
Embodiment 1: alloying constituent is 5wt%Nb, and all the other are Cu.Get purity 〉=99.95%, mean particle size is Cu powder 950g and purity 〉=99.90% of 10～15 μ m, and the Nb powder 50g of mean particle size＜5 μ m mixes the back ball milling;
Milling parameters is: vacuum tightness (5～6) * 10
-2Pa, ratio of grinding media to material 15: 1, rotational speed of ball-mill 250rpm, ball milling time 40h; Make the strong molten and inner Cu-Nb nanometer crystal alloy powder that contains a large amount of less than 5nm disperse Nb or NbO particle;
Then, Cu-Nb nanometer crystal alloy powder is annealed under hydrogen shield atmosphere;
Hydrogen shield atmosphere parameter and annealing is: 600 ℃ of temperature, soaking time 1.0h; Make CuO, Cu in the Cu-Nb powdered alloy behind the ball milling
2O is reduced to Cu;
Subsequently, add the boron powder that accounts for Cu-Nb nanometer crystal alloy powder total amount 50ppm in the Cu-Nb nanometer crystal alloy powder after annealing, after mixing, in the vacuum hotpressing machine, carry out hot pressed sintering, make oxygen level≤11ppm, ingot blank relative density and be 98% the metallurgical billet of Cu-Nb;
The hot-pressing sintering technique parameter is: vacuum tightness 10
-2～10
-3Pa, 800 ℃ of temperature, pressure 25MPa, hot pressing time 2h; By the online secondary reduction of solid reductant vacuum hotpressing, can further remove the residual oxygen that remains in the alloy; Prepared alloy ingot blank is carried out annealing in hydrogen atmosphere expansion test, annealing in hydrogen atmosphere expansion data results sees Table 1, and visible " 600 ℃ of online secondary reductions of hydrogen reducing deoxidation+solid reductant (boron powder) vacuum hotpressing " method that adopts can prevent the intumescent generation of ingot blank annealing in hydrogen atmosphere effectively.
Then, under the high pure nitrogen protection of purity＞99.999%, Cu-Nb powder metallurgy billet is added hot extrusion and make the thick extruding slab of 2mm;
The hot extrusion technique parameter is: 800 ℃ of temperature, and the mould temperature is 450 ℃ during hot extrusion, extrusion ratio 15: 1;
With the extruding slab of gained carry out pass deformation be 10% cold roller and deformed, when total deformation reaches 34%～35%, cold rolling material is carried out stress relief annealing down in high pure nitrogen (purity＞99.999%) protection, 650 ℃ of annealing temperatures are incubated 30min; Repeat above-mentioned steps, finally make thick 0.1mm, the band of wide 35mm.The alloy property data that record see Table 2, have also listed the corresponding performance of card thick forest alloy in the table 2, and visible Cu-5wt%Nb alloy various aspects of performance all is better than card thick forest alloy.
Table 1.
| Hot pressing condition | Sample size (mm) before the annealing in hydrogen atmosphere | Sample size (mm) behind 850 ℃ of annealing in hydrogen atmospheres | Swell increment (mm) |
| 850 ℃ of 2h, 30MPa, argon shield | ??φ59.110 | ??φ59.140 | ??0.010 |
| ??850℃2h，30MPa，10 -5The Torr vacuum | ??φ59.090 | ??φ59.095 | ??0.005 |
| ??850℃2h，30MPa，10 -5Torr vacuum (adding 200ppm boron) | ??φ59.092 | ??φ59.092 | ??0.000 |
Table 2
Embodiment 2: alloying constituent is 7wt%Nb, and all the other are Cu.Processing step is identical with embodiment 1, make thick 0.3mm, the band of wide 35mm, the alloy property data that record see Table 3, also listed the corresponding performance of Cu-9.0Ni-1.4Al alloy in the table 3, visible Cu-7wt%Nb alloy various aspects of performance all is better than alloy Cu-9.0Ni-1.4Al alloy.
The concrete processing parameter of present embodiment is:
Milling parameters: purity＞99.999% high-purity argon gas protection, ratio of grinding media to material 17: 1, rotational speed of ball-mill 300rpm, ball milling time 50h;
Hydrogen shield atmosphere parameter and annealing: 600 ℃ of temperature, soaking time 1.5h;
Hot-pressing sintering technique parameter: vacuum tightness 10
-2～10
-3Pa, 850 ℃ of temperature, pressure 28MPa, hot pressing time 2h;
The hot extrusion technique parameter: the mould temperature is 500 ℃ during hot extrusion, extrusion ratio 15: 1;
Cold rolling pass deflection: 9%;
Stress relief annealing processing parameter: 700 ℃ of temperature, soaking time 40min;
Table 3
Embodiment 3: alloying constituent is 10wt%Nb, and all the other are Cu.Processing step is identical with embodiment 1, make thick 0.5mm, the band of wide 35mm, the alloy property data that record see Table 4, also listed the corresponding performance of Cu-15Ni-8.0Sn alloy in the table 4, visible Cu-10wt%Nb alloy strength and electric conductivity all are better than the Cu-15Ni-8.0Sn alloy.Accompanying drawing 2 is the TEM tissue and the corresponding electron diffraction pattern of present embodiment alloy, and as can be seen from Figure 2, alloy strengthening particle of the present invention is Nb, and its size is about 5～10nm, and the pinning dislocation makes this alloy have quite high stress relaxation-resistant ability strongly.
The concrete processing parameter of present embodiment is:
Milling parameters: vacuum tightness (5～6) * 10
-2Pa, ratio of grinding media to material 20: 1, rotational speed of ball-mill 350rpm, ball milling time 50h;
Hydrogen shield atmosphere parameter and annealing: 650 ℃ of temperature, soaking time 1.5h;
Hot-pressing sintering technique parameter: vacuum tightness 10
-2～10
-3Pa, 900 ℃ of temperature, pressure is 30MPa, hot pressing time 2h;
The hot extrusion technique parameter: the mould temperature is 550 ℃ during hot extrusion, extrusion ratio 15: 1;
Cold rolling pass deflection: 8%;
Stress relief annealing processing parameter: 750 ℃ of temperature, soaking time 60min;
Table 4
Claims (1)
1. the preparation method of a nano dispersion reinforced elastic Cu-Nb alloy may further comprise the steps:
The first step: preparation hypoxemia level Cu-Nb alloy ingot blank
1, presses each weight percentages of components of Cu-Nb alloy, get purity 〉=99.95% respectively, mean particle size is Cu powder and purity 〉=99.90% of 10～15 μ m, the Nb powder of mean particle size＜5 μ m mixes, it in vacuum tightness ball milling under the argon gas atmosphere protection of (5～6) * 10-2Pa or purity＞99.999%, ratio of grinding media to material (15～20): 1, rotational speed of ball-mill 250～350rpm, ball milling time 40～50h makes the strong molten and inner Cu-Nb nanometer crystal alloy powder that contains a large amount of less than 5nm disperse Nb or NbO particle;
2, with Cu-Nb nanometer crystal alloy powder under the hydrogen shield atmosphere in 600～650 ℃ stove, insulation 1.0～1.5h carries out hydrogen shield annealing; Add the boron powder that accounts for Cu-Nb nanometer crystal alloy powder total amount 50～300ppm in the Cu-Nb nanometer crystal alloy powder after annealing, after mixing, in the vacuum hotpressing machine, carry out hot pressed sintering, make the metallurgical billet of Cu-Nb of oxygen level≤11ppm; The hot-pressing sintering technique parameter is: vacuum tightness 10-2～10-3Pa, 800～850 ℃ of temperature, pressure 25～30MPa, hot pressing time 2h;
Second step: hot extrusion and cold-rolling process prepare the elasticity band
1, under the high pure nitrogen protection of purity＞99.999% Cu-Nb powder metallurgy billet is heated to 800～900 ℃, hot extrusion makes the extruding slab; Mould temperature 〉=450 ℃ during hot extrusion, extrusion ratio 〉=15: 1;
2, the extruding slab of gained is carried out pass deformation be 8%～10% cold roller and deformed, when total deformation reaches 34%～35%, cold rolling material is carried out stress relief annealing, 600～750 ℃ of annealing temperatures, soaking time 30～60min under the high pure nitrogen protection of purity＞99.999%; Repeat above-mentioned steps, finally make the cold rolling elasticity band of high precision of thick 0.1～0.5mm.
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| CN104032152A (en) * | 2014-05-14 | 2014-09-10 | 苏州金江铜业有限公司 | Preparation method for Cu-Nb nano-dispersion reinforced copper alloy |
| CN106399742A (en) * | 2016-06-08 | 2017-02-15 | 中国计量学院 | Cu-NbC nanometer dispersion strengthened copper alloy and preparation method thereof |
| CN106676313A (en) * | 2016-12-28 | 2017-05-17 | 北京有色金属研究总院 | Preparation method of high-intensity and high-conductivity Cu-Nb alloy billet |
| CN106756141A (en) * | 2016-12-28 | 2017-05-31 | 北京有色金属研究总院 | The gas shield solid-liquid mixing coagulation system of Cu Nb in-situ composites |
| CN108242310A (en) * | 2018-01-10 | 2018-07-03 | 海安县巨力磁材有限责任公司 | A kind of preparation method of magnetic material |
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| CN104032152A (en) * | 2014-05-14 | 2014-09-10 | 苏州金江铜业有限公司 | Preparation method for Cu-Nb nano-dispersion reinforced copper alloy |
| CN106399742A (en) * | 2016-06-08 | 2017-02-15 | 中国计量学院 | Cu-NbC nanometer dispersion strengthened copper alloy and preparation method thereof |
| CN106399742B (en) * | 2016-06-08 | 2018-11-30 | 中国计量学院 | A kind of nano dispersion reinforced copper alloy of Cu-NbC and preparation method thereof |
| CN106676313A (en) * | 2016-12-28 | 2017-05-17 | 北京有色金属研究总院 | Preparation method of high-intensity and high-conductivity Cu-Nb alloy billet |
| CN106756141A (en) * | 2016-12-28 | 2017-05-31 | 北京有色金属研究总院 | The gas shield solid-liquid mixing coagulation system of Cu Nb in-situ composites |
| CN106676313B (en) * | 2016-12-28 | 2018-07-17 | 北京有色金属研究总院 | A kind of preparation method of high-strength high-conductivity Cu-Nb alloy blanks |
| CN106756141B (en) * | 2016-12-28 | 2018-08-28 | 北京有色金属研究总院 | The gas shield solid-liquid mixing coagulation system of Cu-Nb in-situ composites |
| CN108242310A (en) * | 2018-01-10 | 2018-07-03 | 海安县巨力磁材有限责任公司 | A kind of preparation method of magnetic material |
| CN110355371A (en) * | 2019-06-21 | 2019-10-22 | 延安速源节能科技有限公司 | A kind of preparation method of highly conductive Cu-Zn alloy |
| CN112831703A (en) * | 2020-12-30 | 2021-05-25 | 南方科技大学 | Niobium-copper alloy material and preparation method thereof |
| CN113969364A (en) * | 2021-09-10 | 2022-01-25 | 中南大学 | High-strength high-conductivity copper-niobium alloy and preparation method thereof |
| CN113969364B (en) * | 2021-09-10 | 2022-05-03 | 中南大学 | High-strength high-conductivity copper-niobium alloy and preparation method thereof |
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