CN104032152A - Preparation method for Cu-Nb nano-dispersion reinforced copper alloy - Google Patents
Preparation method for Cu-Nb nano-dispersion reinforced copper alloy Download PDFInfo
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Abstract
The invention relates to a powder metallurgy material, and discloses a preparation method for Cu-Nb nano-dispersion reinforced copper alloy. The preparation method comprises: putting Cu powder and Nb powder into a vacuum glove box full with high-purity hydrogen, mixing uniformly, then putting in a ball-milling tank and completely sealing the ball-milling tank, then taking out the ball-milling tank from the glove box, and performing ball milling on a ball mill, so as to prepare a supersaturated Cu-Nb nanocrystal powder; and deflating a vacuum furnace, mixing the supersaturated Cu-Nb nanocrystal powder with proper amount of a reducing agent boron powder and putting in a mold, putting the mold into the vacuum hot-pressing furnace, vacuumizing and introducing circulation water, setting a heating temperature, when the vacuum furnace has a certain vacuum degree, starting to heat, when the set temperature is reached, starting to sintering, after pressurization sintering is performed, starting to cool, keeping vacuumizing and introducing circulation water, and taking out the material, so as to obtain the target product. The prepared Cu-Nb nanocrystal powder has the hardness almost exceeding the hardness of present all copper alloy, and prepared double-nanometer-structure alloy billets show excellent comprehensive performances such as high strength and high electric conductivity.
Description
Technical field
The invention belongs to mmaterial technical field, relate to the preparation of nano dispersion reinforced copper alloy, be specifically related to the preparation method of the nano dispersion reinforced copper alloy of a kind of Cu-Nb.
Background technology
Dispersion strengthening copper alloy (Dispersion Strengthened Copper, be called for short DSC) be the copper-based material with good comprehensive physical mechanical property, there is higher specific tenacity, specific modulus, good thermal conductivity, electroconductibility, wear resistance, high-temperature behavior, lower thermal expansivity, the over-all propertieies such as higher dimensional stability.Yield strength and the tensile strength of dispersion-strengthened Cu are high, even after annealing, still possess most of yield strength, annealing can improve the ductility of copper alloy, but because the yield strength retention of dispersion-strengthened Cu is high, therefore in highly conc copper alloy, the dispersion-strengthened Cu yield strength of work hardening is the highest.The intensity of dispersion-strengthened Cu can compare favourably with multiple steel, and conductivity is similar to copper.
At present, copper alloy with high strength and high conductivity is because of its good electroconductibility, high intensity and superior high-temperature behavior, being considered to the utmost point has the new function material of development potentiality and application prospect, at super large-scale integration lead frame, high impulse magnetic field conductors, radar, high-power military microwave tube for defence and military, for high-speed rail transportation, numerous high-technology fields such as aerial condutor, resistance welding electrode and conticaster crystallizer are widely used.Obviously, development copper alloy with high strength and high conductivity is all significant to national economy, hi-tech development and national defense construction.
The matter of utmost importance that exploitation copper alloy with high strength and high conductivity faces is to solve copper alloy intensity and this conflict of specific conductivity, improves copper alloy intensity and often will reduce its specific conductivity.According to Norbury-Linde rule, the lattice lattice distortion causing in Cu matrix due to solute atoms solid solution is stronger to unbound electron scattering process, therefore alloying element add the specific conductivity that all can reduce to some extent copper, this makes traditional solution strengthening be difficult to meet the requirement of copper alloy high-strength highly-conductive.Therefore, must adopt special schedule of reinforcement significantly not reducing on the basis of copper matrix electric conductivity, alloy strength is significantly improved.The schedule of reinforcement adopting at present mainly contains: precipitation strength, dispersion-strengthened, fiber strengthening, refined crystalline strengthening and deformation processed composite strengthening etc.
At present, the preparation method of copper alloy with high strength and high conductivity mainly contains: powder metallurgic method, internal oxidation, mechanical alloying method, rapid solidification method and large plastometric set etc.
Existing copper alloy with high strength and high conductivity and technology of preparing thereof also exist many problems, for example material property can't meet the requirement of growing high and new technology, complicated process of preparation, production process is difficult to control, production cost is higher, product performance are unstable etc., and these problems have seriously restricted future development and the application of copper alloy with high strength and high conductivity.
Summary of the invention
In view of this, the object of the present invention is to provide the preparation method of simple, the easy to operate nano dispersion reinforced copper alloy of Cu-Nb of a kind of processing method, the deficiency existing to improve existing preparation method, prepares the dispersion strengthening copper alloy that performance is more excellent.
Mechanical alloying method also claims high-energy ball milling method, is a kind of non-equilibrium new and high technology of preparing powdered alloy of first being developed under laboratory condition by people such as Benjamin for 1966.This technique is applied to the preparation of oxide dispersion intensifying (ODS) alloy the earliest, and the industrialization that has realized ODS alloy by INCO company is subsequently produced.Nineteen eighty-three, it is non-crystaline amorphous metal that American scientist professor Koch takes the lead in having prepared Ni-Nb with Mechanic Alloying Technology, has caused physicist and powder metallurgy scholar's extensive attention, has worldwide started thus the climax of mechanical alloying research.
The ultimate principle of mechanical alloying method is that the powder stock mixing is by a certain percentage sealed in ball grinder together with abrading-ball, by high speed rotating or the vibration of ball mill, make abrading-ball obtain enough kinetic energy so that powder is carried out to strong stirring, collision and grinding, make powder particle experience distortion repeatedly, cold welding, fracture, seam and again shattering process again, phase mutual diffusion occurring between powder atom or carry out solid state reaction formation grain-size is nano level powdered alloy, again by selecting suitable press process technique, finally prepare and under normal condition, be difficult to synthetic alloy material.In addition, mechanical alloying method also has technique simple economy, and operation composition is the advantage such as adjustable continuously.In recent years, mechanical alloying method, as a kind of preparation technology who realizes the horizontal alloying of atom level between constituent element, is applied to the preparation of high-intensity high-conductivity copper alloy gradually, has very vast potential for future development.
The principle of contriver based on above-mentioned, selects its process parameter, mainly comprises rotating speed, ball milling temperature and the Ball-milling Time etc. of ball-milling material, ball loadings, ratio of grinding media to material, ball mill.
For achieving the above object, the invention provides following technical scheme:
The preparation method of the nano dispersion reinforced copper alloy of Cu-Nb of the present invention, comprises the steps:
Cu powder and Nb powder are packed in the vacuum glove box that is full of high-purity hydrogen, after mixing, put into ball grinder, to after ball grinder sealing completely, from glove box, take out again, in ball mill, ratio of grinding media to material 5 ~ 20:1, rotational speed of ball-mill 200 ~ 350rpm, ball milling 1 ~ 100 hour, prepares supersaturation Cu-Nb manocrystalline powders; Vacuum oven venting, the borane reducing agent powder that the supersaturation Cu-Nb manocrystalline powders mixing of gained is accounted for to its content 50 ~ 300ppm packs mould into and puts into vacuum hotpressing stove, vacuumizes and logical recirculated water, sets 600 ~ 900 DEG C of Heating temperatures, when reaching 10
-5when torr, start heating, while reaching design temperature, under 20 ~ 30Mpa, start pressure sintering, start cooling after pressure sintering 1 ~ 3h, keep vacuumizing and logical recirculated water, feeding, obtains target product.
In technique scheme, the mass ratio of described Cu powder and Nb powder is (100-X): X, X=5 ~ 20.
Preferably, described Cu powder powder size is less than 300 orders, and described Nb powder powder size is less than 300 orders.
In technique scheme, described ball grinder and abrading-ball are that quenching stainless material is made.
Preferably, ratio of grinding media to material 15:1 when ball milling, rotational speed of ball-mill 300rpm, Ball-milling Time 40 ~ 100 hours.
Preferably, 850 DEG C of temperature, under 30Mpa, start pressure sintering, after pressure sintering 2h, start cooling.
In the Cu-Nb manocrystalline powders that method of the present invention makes, Cu phase average grain-size can reach 7 ~ 13nm, and due to the acting in conjunction of solution strengthening, refined crystalline strengthening, twin boundary strengthening and strain hardening, Cu-Nb Nanocrystalline Solid Solution hardness HV can reach 367 ~ 490Kgf/mm
2, almost exceeded the hardness of current all copper alloys.The double nano structural alloy ingot blank making, its salient features can reach hardness HV=364Kgf/mm
2, relative conductivity=52%IACS, has shown excellent high strength and high over-all properties of conducting electricity.
Embodiment
To the technical scheme in the embodiment of the present invention be described in detail below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiment.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite of not making creative work, belongs to the scope of protection of the invention.
Experiment material used in following embodiment, if no special instructions, all can be bought and be obtained by routine biochemistry reagent shop, and the granularity of Cu powder powder and Nb powder powder is all less than 300 orders, and ball grinder and abrading-ball are that quenching stainless material is made.
Embodiment 1
95kg Cu powder and 5kg Nb powder are packed in the vacuum glove box that is full of high-purity hydrogen, after mixing, put into ball grinder, to after ball grinder sealing completely, from glove box, take out again, in ball mill, ratio of grinding media to material 20:1, rotational speed of ball-mill 200rpm, ball milling 100 hours, prepares supersaturation Cu-Nb manocrystalline powders; Vacuum oven venting, the borane reducing agent powder that the supersaturation Cu-Nb manocrystalline powders mixing of gained is accounted for to its content 50ppm packs mould into and puts into vacuum hotpressing stove, vacuumizes and logical recirculated water, sets 600 DEG C of Heating temperatures, when reaching 10
-5when torr, start heating, while reaching design temperature, under 20Mpa, start pressure sintering, start cooling after pressure sintering 3h, keep vacuumizing and logical recirculated water, feeding, obtains target product.
Embodiment 2
90kg Cu powder and 10kg Nb powder are packed in the vacuum glove box that is full of high-purity hydrogen, after mixing, put into ball grinder, to after ball grinder sealing completely, from glove box, take out again, in ball mill, ratio of grinding media to material 15:1, rotational speed of ball-mill 250rpm, ball milling 60 hours, prepares supersaturation Cu-Nb manocrystalline powders; Vacuum oven venting, the borane reducing agent powder that the supersaturation Cu-Nb manocrystalline powders mixing of gained is accounted for to its content 100ppm packs mould into and puts into vacuum hotpressing stove, vacuumizes and logical recirculated water, sets 700 DEG C of Heating temperatures, when reaching 10
-5when torr, start heating, while reaching design temperature, under 25Mpa, start pressure sintering, start cooling after pressure sintering 2h, keep vacuumizing and logical recirculated water, feeding, obtains target product.
Embodiment 3
85kg Cu powder and 15kg Nb powder are packed in the vacuum glove box that is full of high-purity hydrogen, after mixing, put into ball grinder, to after ball grinder sealing completely, from glove box, take out again, in ball mill, ratio of grinding media to material 10:1, rotational speed of ball-mill 300rpm, ball milling 20 hours, prepares supersaturation Cu-Nb manocrystalline powders; Vacuum oven venting, the borane reducing agent powder that the supersaturation Cu-Nb manocrystalline powders mixing of gained is accounted for to its content 200ppm packs mould into and puts into vacuum hotpressing stove, vacuumizes and logical recirculated water, sets 800 DEG C of Heating temperatures, when reaching 10
-5when torr, start heating, while reaching design temperature, under 30Mpa, start pressure sintering, start cooling after pressure sintering 1h, keep vacuumizing and logical recirculated water, feeding, obtains target product.
Embodiment 4
80kg Cu powder and 20kg Nb powder are packed in the vacuum glove box that is full of high-purity hydrogen, after mixing, put into ball grinder, to after ball grinder sealing completely, from glove box, take out again, in ball mill, ratio of grinding media to material 5:1, rotational speed of ball-mill 350rpm, ball milling 1 hour, prepares supersaturation Cu-Nb manocrystalline powders; Vacuum oven venting, the borane reducing agent powder that the supersaturation Cu-Nb manocrystalline powders mixing of gained is accounted for to its content 300ppm packs mould into and puts into vacuum hotpressing stove, vacuumizes and logical recirculated water, sets 900 DEG C of Heating temperatures, when reaching 10
-5when torr, start heating, while reaching design temperature, under 25Mpa, start pressure sintering, start cooling after pressure sintering 2h, keep vacuumizing and logical recirculated water, feeding, obtains target product.
Embodiment 5
90kg Cu powder and 10kg Nb powder are packed in the vacuum glove box that is full of high-purity hydrogen, after mixing, put into ball grinder, to after ball grinder sealing completely, from glove box, take out again, in ball mill, ratio of grinding media to material 15:1, rotational speed of ball-mill 300rpm, ball milling 40 hours, prepares supersaturation Cu-Nb manocrystalline powders; Vacuum oven venting, the borane reducing agent powder that the supersaturation Cu-Nb manocrystalline powders mixing of gained is accounted for to its content 200ppm packs mould into and puts into vacuum hotpressing stove, vacuumizes and logical recirculated water, sets 850 DEG C of Heating temperatures, when reaching 10
-5when torr, start heating, while reaching design temperature, under 30Mpa, start pressure sintering, start cooling after pressure sintering 2h, keep vacuumizing and logical recirculated water, feeding, obtains target product.
In those skilled in the art, obviously the invention is not restricted to the details of above-mentioned example embodiment, and in the situation that not deviating from spirit of the present invention or essential characteristic, can realize the present invention with other specific form.Therefore, no matter from which point, all should regard embodiment as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, is therefore intended to all changes that drop in the implication and the scope that are equal to important document of claim to include in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but be not that each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should make specification sheets as a whole, and the technical scheme in each embodiment also can, through appropriately combined, form other embodiments that it will be appreciated by those skilled in the art that.
Claims (6)
1. a preparation method for the nano dispersion reinforced copper alloy of Cu-Nb, is characterized in that, comprises the steps:
Cu powder and Nb powder are packed in the vacuum glove box that is full of high-purity hydrogen, after mixing, put into ball grinder, to after ball grinder sealing completely, from glove box, take out again, in ball mill, ratio of grinding media to material 5 ~ 20:1, rotational speed of ball-mill 200 ~ 350rpm, ball milling 1 ~ 100 hour, prepares supersaturation Cu-Nb manocrystalline powders; Vacuum oven venting, the borane reducing agent powder that the supersaturation Cu-Nb manocrystalline powders mixing of gained is accounted for to its content 50 ~ 300ppm packs mould into and puts into vacuum hotpressing stove, vacuumizes and logical recirculated water, sets 600 ~ 900 DEG C of Heating temperatures, when reaching 10
-5when torr, start heating, while reaching design temperature, under 20 ~ 30Mpa, start pressure sintering, start cooling after pressure sintering 1 ~ 3h, keep vacuumizing and logical recirculated water, feeding, obtains target product.
2. preparation method according to claim 1, is characterized in that: the mass ratio of described Cu powder and Nb powder is (100-X): X, X=5 ~ 20.
3. preparation method according to claim 1 and 2, is characterized in that: described Cu powder powder size is less than 300 orders, and described Nb powder powder size is less than 300 orders.
4. preparation method according to claim 1, is characterized in that: described ball grinder and abrading-ball are that quenching stainless material is made.
5. preparation method according to claim 1, is characterized in that: ratio of grinding media to material 15:1 when ball milling, rotational speed of ball-mill 300rpm, Ball-milling Time 40 ~ 100 hours.
6. preparation method according to claim 1, is characterized in that: 850 DEG C of temperature, under 30Mpa, start pressure sintering, start cooling after pressure sintering 2h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN106884115A (en) * | 2017-04-19 | 2017-06-23 | 德阳鑫晶科技有限公司 | The preparation method of the magnetic artillery with high connductivity and resistance to high temperature oxidation |
| CN111101010A (en) * | 2019-12-26 | 2020-05-05 | 浙江杭机新型合金材料有限公司 | High-strength high-conductivity copper-niobium alloy material and preparation method thereof |
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| CN101717872A (en) * | 2009-12-21 | 2010-06-02 | 中南大学 | Method for preparing nano dispersion reinforced elastic Cu-Nb alloy |
| CN101818273A (en) * | 2010-04-14 | 2010-09-01 | 中南大学 | Method for preparing Cu-Nb alloy with high strength, high conductivity and high-temperature softening resistance |
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Patent Citations (2)
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| CN101717872A (en) * | 2009-12-21 | 2010-06-02 | 中南大学 | Method for preparing nano dispersion reinforced elastic Cu-Nb alloy |
| CN101818273A (en) * | 2010-04-14 | 2010-09-01 | 中南大学 | Method for preparing Cu-Nb alloy with high strength, high conductivity and high-temperature softening resistance |
Non-Patent Citations (1)
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| 雷若姗，汪明朴，郭明星，李周，曹玲飞，唐宁: "机械合金化制备Cu-Nb纳米弥散强化铜合金的研究", 《材料导报》, vol. 21, 31 May 2007 (2007-05-31), pages 22 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN106884115A (en) * | 2017-04-19 | 2017-06-23 | 德阳鑫晶科技有限公司 | The preparation method of the magnetic artillery with high connductivity and resistance to high temperature oxidation |
| CN111101010A (en) * | 2019-12-26 | 2020-05-05 | 浙江杭机新型合金材料有限公司 | High-strength high-conductivity copper-niobium alloy material and preparation method thereof |
| CN111101010B (en) * | 2019-12-26 | 2021-08-17 | 浙江杭机新型合金材料有限公司 | High-strength high-conductivity copper-niobium alloy material and preparation method thereof |
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Application publication date: 20140910 |