CN1940103A - Cu.TiB nano-diffusion alloy and its production - Google Patents
Cu.TiB nano-diffusion alloy and its production Download PDFInfo
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- CN1940103A CN1940103A CN 200510032207 CN200510032207A CN1940103A CN 1940103 A CN1940103 A CN 1940103A CN 200510032207 CN200510032207 CN 200510032207 CN 200510032207 A CN200510032207 A CN 200510032207A CN 1940103 A CN1940103 A CN 1940103A
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Abstract
This invention relates to a kind of Cu-TiB2 alloy and its preparation method. Taking Cu-Ti and Cu-B as the centre alloy, melting the centre alloy respectively and overheating them till 1300DEG C-1400DEG C, mixing the two melt to take original place reaction, making the uniformity compound body which is composed of the TiB2 nanometer particle and pure cupper fused mass, freezing the compound body quickly with the method of jetting deposition, manufacturing the Cu-TiB2 alloy base ingot , producing the Cu-TiB2 alloy finished product. The alloy in this invention compares with no oxygen copper, have these advantages that it has high intensity, it resists high temperature and its function of anneal and softening are good , whose sigma0.2 is 3-12 times than no oxygen copper, the temperature of the anneal softening is over 900DEG C, the electric conduction rate may arrive at 95% IACS, the electric conduction rate of the high concentration Cu-TiB2 alloy may arrive at 75% IACS , comparing with these deposition strengthening alloys such as the Cu-Fe-P system, Cu-Ni-Si system, Cu-Cr-Zr system , the Cu-TiB2 alloy has the functions that it has higher electric conduction and it resists high temperature as well as the good function of anneal and softening.
Description
Technical field
The present invention relates to a kind of Cu-TiB
2Alloy And Preparation Method, this copper alloy have high strength, high conduction, high temperature resistance annealing softening characteristic, can be applicable to fields such as electrovacuum, resistance welding electrode, high-voltage switch gear, electron and electrician, nuclear technique.
Background technology
In fields such as microwave technology, microelectronics, electrician, automobile making, metallurgy, nuclear technique, the copper alloy of a kind of high strength of widespread demand, high conduction, high temperature resistance annealing softening characteristic, it is a critical material of making 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 etc.Though fine copper electroconductibility height (98～102%IACS), the too low (σ of intensity
0.250MPa only); Though serial copper alloys such as Cu-Fe-P, Cu-Ni-Si, Cu-Cr-Zr have the characteristic of high strength, high conduction, they are ageing strengthening type alloys, can occur the overaging phenomenon in temperature during greater than 500 ℃, and annealing softening promptly takes place.When particularly temperature was higher than 600 ℃, this class alloy not only reduced because of sharply softening intensity, and can sharply reduce because of the molten electroconductibility that causes of returning of precipitation particles, thereby made the characteristic of alloy forfeiture high-strength highly-conductive.Cu-Al
2O
3Alloy is the nano dispersion reinforced copper alloy that a class has high strength, high conduction, high temperature resistance annealing softening excellent specific property, but its enhanced particles Al
2O
3Non-conductive.This point is particularly unfavorable in the application in microelectronic and electrovacuum field, and it not only influences with the electrical spark of the accurate device of its making or electron beam processing, and can cause the micro element regional area electroconductibility interruption with its making, even can not work.Therefore the material that needs to make this class device not only has Cu-Al
2O
3High strength, high conduction and high temperature resistance annealing softening characteristic that alloy is excellent equally, and need its enhanced particles also to have electroconductibility, be beneficial to the accurate electrospark machining or the electron beam processing of micro element and prevent the interruption of micro element microcell electroconductibility.
In-situ reaction is all adopted in the preparation of nano dispersion reinforced copper alloy usually, prepares Cu-Al as internal oxidation
2O
3Alloy, mechanical alloying method prepare Cu-Al
2O
3, Cu-TiB
2, Cu-Nb alloy etc.Internal oxidation is to utilize the control oxygen partial pressure to make interior oxidation reaction in takes place in the Cu-Al alloy powder, generates Al in the copper powder matrix
2O
3Nanoparticle.This method prepares Cu-Al
2O
3Alloy prior is quite complicated, comprise: the Cu-Al alloy melting, dust, oxygenant preparation, batch mixing, interior oxidation, reduction, isostatic cool pressing, vacuum sintering, jacket hot extrusion, cold machine-shaping etc., process is difficult to control, and both at home and abroad producer seldom has and can really grasp its gordian technique.Mechanical alloying method is to utilize high-energy ball milling to make two or more alloy powder generation reaction in generate nanoparticle, as high-energy ball milling Cu, Ti, B powder, and by subsequent heat treatment or hot-work formation Cu-TiB
2Alloy.
Summary of the invention
Purpose of the present invention is invented a kind of Cu-TiB
2Nano dispersion reinforced copper alloy and two melt in situ reaction method for preparing thereof, this copper alloy have high strength, high conduction, high temperature resistance annealing softening characteristic.
A kind of Cu-TiB
2Alloy, its weight consists of: 0.20～3.0%TiB
2, all the other are copper.
Cu-TiB
2Nano dispersion reinforced process for producing copper alloy adopts Cu-Ti and Cu-B as master alloy, and after master alloy is melted respectively and being superheated to 1300 ℃～1400 ℃, two melt-mixing adopt 10
5～2 * 10
5High-pressure inert gas (the high-purity N of Pa
2Gas or Ar gas), make alloy melt is pressed into reaction chamber from two pipelines respectively, reaction in takes place when collision mixes mutually.Make two melt-mixing generation reaction ins, generate TiB
2The homogeneous mixture of nanoparticle and fine copper melt, with the method rapid condensation of this mixture with jet deposition, the condition of jet deposition is: pressure: 3 * 10
5～6 * 10
5Pa, atomizing gas: N
2Gas or Ar gas are made Cu-TiB
2The alloy billet is processed into Cu-TiB
2The alloy finished product.
A kind of preparation Cu-TiB
2Two melt in situ reaction units of alloy billet, mainly comprise: two furnace chambers and a spraying chamber, the bottom in furnace chamber and spraying chamber is respectively arranged with bleeds to cavity, the hole of supplying gas, in furnace chamber, be provided with the induction furnace that can melt master alloy, the two melt in situ reactors of " Y " type are arranged between two induction furnaces, be used to carry the interior master alloy of induction furnace and carry out reaction in, valve is set on two pipelines in the two melt in situ reactor node tops of " Y " type is used to control the flow of alloy melt and the atmospheric pressure state (vacuum state or high-pressure aerated state) in the control furnace chamber, on the vertical ducting of the two melt in situ reactor node bottoms of " Y " type, Vltrasonic device is set, promptly be provided with spraying gun at the end of the two melt in situ reactors of " Y " type with the contact position in spraying chamber, the spraying gun below is provided with rotatable liftable substrate that supports the jet deposition billet and the guide deflection sheave that draws the billet motion, between furnace chamber and the spraying chamber dividing plate is installed, supports furnace chamber and sealing spraying chamber.
Alloy of the present invention is compared with oxygen free copper (C10100, TU1), has intensity height, advantage that high temperature resistance annealing softening performance is high.Look TiB
2The particle content difference, its σ
0.2Comparable oxygen free copper is high 3～12 times, and anti-annealing softening temperature can be up to more than 900 ℃, and electric conductivity can reach 95%IACS, very near oxygen free copper, and high density Cu-TiB
2The 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-TiB
2It is obviously high that alloy conductive is wanted, and do not have intensity that overaging and high temperature Hui Rong cause and the electric conductivity problem that sharply descends.With Cu-Al
2O
3Disperse copper is compared, and the two intensity, electroconductibility, high temperature resistance annealing softening performance are suitable, but TiB
2Particle has electroconductibility, has avoided Cu-Al
2O
3Alloy is difficult to carry out the processing of accurate electrical spark or electron beam, and problem such as the microcell conduction is discontinuous.On the preparation method, to compare with internal oxidation, two melt in situ reaction methods are a kind of short process making methods, have to produce that equipment is simple, preparation cost is low, middle-chain is few, be easy to series of advantages such as control.
Description of drawings
Fig. 1: process flow sheet of the present invention;
Fig. 2: two melt in situ reaction unit figure;
Fig. 3: Cu-TiB
2TiB in the alloy
2Particle TEM photo (a), and respective electronic diffraction pattern (b)
Embodiment
Below in conjunction with accompanying drawing the two melt in situ reaction units of the present invention are described further.Two melt in situ are reflected in the hybrid reaction chamber carries out, and its principle of work is shown in Fig. 2.Two induction furnaces 9 about Cu-Ti and Cu-B alloy placed respectively, valve-off 1, and by the injection well 10 of bleeding two furnace chambers 2 are found time, start two induction furnaces 9 simultaneously, the fusing master alloy.Keep vacuum tightness to 10 in the melting process
-1Near the Pa, arrive 1300 ℃～1400 ℃ of design temperatures after, stop to find time, and in two furnace chambers, send into high-purity N by the injection well 10 of bleeding
2Gas or Ar gas make outside chamber internal gas pressure and the chamber identical.Open two valves 1 of two melt in situ reactor 7 tops this moment, start the Vltrasonic device 4 of two melt in situ reactor 7 peripheries, bleed from two respectively simultaneously and send into high pressure gas the injection well 10 melt 3 (Cu-B) and melt 8 (Cu-Ti) are pressed into two melt in situ reactors 7, and make two melts form turbulent flow in the collision of two melt in situ reactor 7 intersections of " Y " type, and the generation reaction in, in the Cu melt, generate TiB
2Nanoparticle.The TiB that carries out and prevent to have generated in the Cu melt for reacting fully
2Particle is grown up, special reaction cavity outer setting at two melt in situ reactors 7 Vltrasonic device 4.Under the effect of high pressure gas, in reaction cavity, finish the Cu-TiB of reaction in
2Mixture enters spraying gun 12 rapidly, with another strand high pressure (3～6 normal atmosphere) N
2Gas or Ar aerosolization, and rapid condensation is deposited as Cu-TiB on the substrate 6 in spraying chamber 14
2Alloy ingot blank 5.Separate by dividing plate 11 and furnace chamber 2 in spraying chamber 14.Not oxidation of alloy when atomizing for making, spraying chamber 14 planted agents elder generation passing hole channel 15 is extracted atmosphere out, and charges into N
2Gas or Ar gas, high pressure gas enter spraying chamber 14 by vent channel 15 discharges during atomizing.Obtain Cu-TiB as stated above
2Alloy ingot blank 5, Cu-TiB
2Alloy ingot blank 5 moves downward by guide deflection sheave 13.Cu-TiB
2Alloy billet 5 is become a useful person through heat, cold working.
Embodiment 1: alloying constituent is TiB
2-0.25wt%, all the other are copper and inevitable impurity.The starting material of preparation alloy are Cu-0.34wt%Ti and Cu-0.17wt%B, with it respectively in two crucibles in device shown in Figure 2 after the fusing, be superheated to 1350 ℃ after, with 2 * 10
5The high pressure high-purity N of Pa
2Gas is pressed into reaction chamber from two pipelines respectively with alloy melt, makes two melts when collision mixes mutually reaction in take place, and generates TiB
2The homogeneous mixture of nanoparticle and fine copper melt, with the method rapid condensation of this mixture with jet deposition, the condition of jet deposition is: pressure: 3 * 10
5～6 * 10
5Pa, atomizing gas: N
2Gas is made Cu-TiB
2The alloy billet, again through hot rolling, make the thin plate of thick 0.30mm after cold rolling.Its salient features sees Table 1, for ease of relatively, has also listed the corresponding performance (two alloys are all through 900 ℃ of annealing in hydrogen atmosphere annealing 0.5h) of TU1 fine copper in the table 1.This routine invention alloy is with preparation microwave tube aperture plate.
The performance of table 1 alloy of the present invention and TU1 fine copper relatively
| σ b(MPa) | σ 0.2(MPa) | δ 5(％) | g(％IACS) | |
| Alloy TU1 of the present invention | 270 190 | 150 45 | 30 40 | 95 100 |
Embodiment 2: alloying constituent is TiB
2-0.5wt%, all the other are copper and inevitable impurity.The starting material of preparation alloy are Cu-0.68wt%Ti, Cu-0.34wt%B, with its respectively in two crucibles in device shown in Figure 2 the fusing back and be superheated to 1350 ℃ after, with 2 * 10
5The high pressure high-purity Ar gas of Pa is pressed into reaction chamber from two pipelines respectively with alloy melt, makes two melts when collision mixes mutually reaction in take place, and generates TiB
2The homogeneous mixture of nanoparticle and fine copper melt, with the method rapid condensation of this mixture with jet deposition, the condition of jet deposition is: pressure: 3 * 10
5～6 * 10
5Pa, atomizing gas: Ar gas, make Cu-TiB
2The alloy billet becomes the bar of Φ 12 through hot extrusion, cold drawing.Its salient features sees Table 2, for ease of relatively, has also listed Cu-0.35wt%Al in the table 2
2O
3The corresponding performance of dispersion strengthening copper alloy (two alloys are all through 900 ℃ of annealing in hydrogen atmosphere annealing 0.5h), as seen both are suitable.Fig. 3 shows this routine invention alloy TEM photo and corresponding electron diffraction pattern, and visible alloy strengthening particle of the present invention is TiB
2, its size is about 10～50nm.
Table 2 alloy of the present invention and Cu-0.35wt%Al
2O
3The dispersion-strengthened Cu performance relatively
| σ b(MPa) | σ 0.2(MPa) | δ 5(％) | g(％IACS) | |
| Alloy Cu-0.35wt%Al of the present invention 2O 3 | 380 385 | 320 310 | 18 20 | 90 90 |
Claims (3)
1. Cu-TiB
2Alloy is characterized in that: weight consists of: 0.20～3.0% TiB
2, all the other are copper.
2. described Cu-TiB of claim 1
2The preparation method, it is characterized in that: adopt Cu-Ti and Cu-B as master alloy, after master alloy is melted respectively and being superheated to 1300 ℃～1400 ℃, make two melt-mixing generation reaction ins, generate TiB
2The homogeneous mixture of nanoparticle and fine copper melt, with the method rapid condensation of this mixture with jet deposition, the condition of jet deposition is: pressure: 3 * 10
5～6 * 10
5Pa, atomizing gas: N
2Gas or Ar gas are made Cu-TiB
2The alloy billet is processed into Cu-TiB
2The alloy finished product.
3. one kind is adopted the described method of claim 2 to prepare the described Cu-TiB of claim 1
2Two melt in situ reaction units of alloy, it is characterized in that: mainly comprise: two furnace chambers and a spraying chamber, the bottom in furnace chamber and spraying chamber is respectively arranged with bleeds to cavity, the hole of supplying gas, in furnace chamber, be provided with the induction furnace that can melt master alloy, the two melt in situ reactors of " Y " type are arranged between two induction furnaces, be used to carry the interior master alloy of induction furnace and carry out reaction in, valve is set on two pipelines in " Y " type reaction in device node top is used to control the flow of alloy melt and the atmospheric pressure state in the control furnace chamber, on the vertical ducting of " Y " type reaction in device node bottom, Vltrasonic device is set, promptly be provided with spraying gun at the end of " Y " type reaction in device with the contact position in spraying chamber, the spraying gun below is provided with rotatable liftable substrate that supports the jet deposition billet and the guide deflection sheave that draws the billet motion, between furnace chamber and the spraying chamber dividing plate is installed, supports furnace chamber and sealing spraying chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100322078A CN100410402C (en) | 2005-09-30 | 2005-09-30 | Cu.TiB nano-diffusion alloy and its production |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100322078A CN100410402C (en) | 2005-09-30 | 2005-09-30 | Cu.TiB nano-diffusion alloy and its production |
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|---|---|
| CN1940103A true CN1940103A (en) | 2007-04-04 |
| CN100410402C CN100410402C (en) | 2008-08-13 |
Family
ID=37958625
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100322078A Expired - Fee Related CN100410402C (en) | 2005-09-30 | 2005-09-30 | Cu.TiB nano-diffusion alloy and its production |
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Assignee: Changsha Zhonggong New Material Co., Ltd. Assignor: Central South University Contract fulfillment period: 2008.9.20 to 2013.9.20 contract change Contract record no.: 2008430000032 Denomination of invention: Cu-TiB#-[2] nano dispersion alloy and preparation method thereof Granted publication date: 20080813 License type: Exclusive license Record date: 20081119 |
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