CN101554685A - High-entropy alloy solder used for welding copper and aluminum and preparation method thereof - Google Patents
High-entropy alloy solder used for welding copper and aluminum and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-entropy alloy solder used for welding copper and aluminum, which comprises the components according to the atomic percent with the total percentage being 100%: 6-14% of Ti, 10-20% of Al, 10-20% of Fe, 15-25% of Cu, 10-18% of Ni, 6-14% of Co, 0.5-4.5% of Sn and 0.03-3.5% of addition element, wherein, the addition element is one selected from Bi, Ga, In or RE. The invention also discloses a preparation method of the high-entropy alloy solder foil, which adopts stepwise smelting technique and a single-roller rapid solidification device to prepare the high-entropy alloy solder foil. The high-entropy alloy solder has good flexibility and is convenient for processing and assembly; when in welding, the high-entropy alloy solder has good metallic matching property with Al and Cu; the soldering seam is good in corrosion-resistant performance, the welding seam is single-phase fcc solid solution tissue, no friable intermetallic compound is generated, and the comprehensive mechanical property of joints can be remarkably improved; the preparation method of the high-entropy alloy solder has simple technique and low manufacturing cost.
Description
Technical field
The invention belongs to technical field of welding materials, relate to a kind of high-entropy alloy solder that is used for soldering copper and aluminium, the invention still further relates to the preparation method of this kind solder alloy.
Background technology
The global rare problem of copper resource has caused the strong interest of international community, it is very urgent to seek the copper substitute, and the electricity of aluminium, thermal property and copper are comparatively approaching, are suitable copper substitution material, China is the state of the rich aluminium of poor copper, and " with aluminium for copper " is the optimal selection of performance china natural resources advantage.The key problem in technology of " with aluminium for copper " is the Welding Problems that solves between aluminium and the copper, the aluminum bronze welding belongs to the welding between the dissimilar metal, its difficulty is bigger, because all there are bigger difference in fusing point, the latent heat of fusion and the linear expansion coefficient etc. of two kinds of metals, and easily react each other and form hard crisp intermetallic compound phase, not only influence the serviceability of joint, and very easily cause fire check, make the making difficulty of copper aluminum metal joint.
Based on existing physical and chemical performance aspect between two kinds of metals than big-difference, should avoid the molten solder between the Cu/Al metal as far as possible, soldering is that mother metal does not melt, after filling metal molten, be full of the gap, and and mother metal between the welding method of dissolving and spreading, be particularly suitable for the welding of foreign material, and weldment distortion is little, equipment is simple, easy and simple to handle, possess the advantage of welding at the scene.The subject matter that the aluminum current copper brazing exists is to use traditional zinc-based solder (Zn-Sn-Cu, Zn-Al-Cu) and aluminium base solder (Al-Si-Mn, Al-Zn-Si) to form meltable fragility Al-CuAl easily in joint
2The cocrystalization compound phase causes strength of joint to reduce.To treat that the indirect soldering of carrying out after weldment surface do plating Ni handles can obviously reduce the generation of intermetallic compound, but this method is difficult to the control of intermetallic compound thickness, formed Cu/Al dissimilar metal joint performance is often unsatisfactory.
Existing a kind of single roller quick solidification apparatus, device is simple, and is easy to use, obtained good application in preparation alloy foil process.In recent years, people use high and new technology and carried out a large amount of research aspect solder Composition Control and forming techniques, prepared the amorphous microcrystalline attitude solder that seam-filling ability is strong, welding temperature is low, the brazing filler metal processing performance obtains very big change, yet the amorphous microcrystalline solder can not solve the joint embrittlement problem that causes because of the intermetallic deposits yields from the source.
Summary of the invention
The object of the present invention is to provide a kind of high-entropy alloy solder that is used for soldering copper and aluminium, this solder alloy can suppress the chemical reaction between the Cu/Al, prevents to form hard crisp intermetallic compound phase CuAl
2, the high performance copper aluminum metal welding point that can obtain to have single-phase face-centered cubic solid solution micro-structural.
Another object of the present invention is to provide the preparation method of above-mentioned solder alloy.
The technical solution adopted in the present invention is, a kind of high-entropy alloy solder that is used for soldering copper and aluminium, be made up of by atomic percent following component: total percentage is 100%, wherein Ti 6%～14%, Al 10%～20%, Fe 10%～20%, Cu 15%～25%, Ni 10%～18%, Co 6%～14%, Sn 0.5%～4.5%, add element 0.03%～3.5%, interpolation element wherein select for use Bi, Ga, In or RE one of them.
Another technical scheme of the present invention is, a kind of above-mentioned preparation method who is used for the high-entropy alloy solder of soldering copper and aluminium, and this method is implemented according to following steps,
Steps A, the molten foundry alloy of joining: with high pure metal Ti, Al, Fe, Cu, Ni, Co, Sn, interpolation element molten joining in the ultrahigh vacuum electric arc furnaces, concrete steps are:
A1, at first various high pure metals are carried out purified treatment with boric anhydride, again according to the good various high pure metals of atomic percent difference weighing: total percentage is 100%, wherein Ti 6%～14%, Al 10%～20%, Fe 10%～20%, Cu 15%～25%, Ni 10%～18%, Co 6%～14%, Sn 0.5%～4.5%, add element 0.03%～3.5%, interpolation element wherein select for use Bi, Ga, In or RE one of them;
A2, with steps A 1 load weighted various high pure metals, the combination of adding element according to Cu-Sn, Cu-Ni, Ti-Al, Fe-Co-is melted respectively and is joined, and obtains four groups of intermediate alloys;
A3, with the molten four groups of intermediate alloys that prepare of steps A 2, add element combinations according to Cu-Sn and Cu-Ni, Ti-Al and Fe-Co-and carry out secondary together and melt and join, obtain two groups of secondary intermediate alloy Cu-Sn-Ni and Ti-Al-Fe-Co-interpolation element;
A4, two groups of secondary intermediate alloy Cu-Sn-Ni that again steps A 3 obtained and Ti-Al-Fe-Co-add element and melt and join, and obtain high entropy foundry alloy;
Step B, use single roller quick solidification apparatus and prepare high-entropy alloy solder, the molten high entropy foundry alloy for preparing of steps A is put into crucible, crucible bottom has slit injector, after the process that " vacuumizes-fill Ar gas " repeatedly 3～5 times, using high-frequency induction equipment to heat high entropy foundry alloy makes its fusing and crosses thermosetting alloy liquid, after 3～5 minutes, open the rotation of driven by motor running roller, roll surface speed is controlled at 5～40m/s, open the Ar air valve immediately, high speed Ar air-flow sprays alloy liquid rapidly, and stream is mapped to the running roller quench solidification of surperficial also moment of rotation at a high speed, throw away along the running roller tangential direction, obtain the high-entropy alloy solder foil.
High-entropy alloy solder of the present invention, the solder flexility is good, is convenient to processing and assembling; When welding with Al, Cu metal matching is good, the brazed seam decay resistance is good, weld seam is single-phase fcc solid solution tissue, compound generation between no brittle metal, the joint comprehensive mechanical performance significantly improves; The preparation method of this kind high-entropy alloy solder, technology is simple, is convenient to make.
Description of drawings
Fig. 1 is the structural representation of the device that uses among the present invention.
Among the figure, 1, little vacuum chamber, 2, crucible, 3, collecting chamber, 4, foil, 5, vacuum chamber, 6, radio-frequency induction coil, 7, single-phase asynchronous motor, 8, running roller, 11, vavuum pump.
The specific embodiment
The present invention is described in detail below in conjunction with the specific embodiment.
High-entropy alloy solder of the present invention, be made up of by atomic percent following component: total percentage is 100%, wherein Ti 6%～14%, Al 10%～20%, Fe 10%～20%, Cu 15%～25%, Ni 10%～18%, Co 6%～14%, Sn 0.5%～4.5%, add element 0.03%～3.5%, interpolation element wherein select for use Bi, Ga, In or RE one of them.
In high-entropy alloy solder composition of the present invention, the composition of each chemical element and content principle of qualification are: obtain the high-entropy alloy brazed seam in order to make weld metal, prevent that the generation of crisp hard intermetallic compound phase from appearring in the Cu/Al joint, guarantee the mechanical performance of brazed joint, it is alloy that high entropy solder pivot is selected the many pivots of Ti-Al-Fe-Cu-Ni-Co, main cause has: in welding process, mother metal is inevitable to the dissolving of solder, so the solder pivot must contain Al, Cu element; The braze ability of aluminium and copper is relatively poor, needs to add active component Ti in the solder; Desire obtains single-phase fcc solid solution brazed seam, should add the alloying element cu and the Ni of face-centred cubic structure; Co and Fe are the main stuffing constituent element; By in alloy, adding Sn and other element (one of Bi, Ga, In or RE), regulate the solder fusing point, improve the solder activity, crystal grain thinning improves joint performance.
Solder alloy of the present invention is used for the soldering of Cu/Al and alloy thereof, because high entropic effect can effectively suppress the chemical reaction between the Cu/Al, prevents to form hard crisp intermetallic compound phase CuAl
2Thereby, obtain high performance copper aluminum metal welding point with single-phase face-centered cubic solid solution micro-structural.
The preparation method of high-entropy alloy solder of the present invention, use single roller quick solidification apparatus to be prepared, this apparatus structure as shown in Figure 1, be included in the copper running roller 8 that is provided with in the vacuum chamber 5 by single-phase asynchronous motor 7 transmissions, directly over running roller 8, be provided with radio-frequency induction coil 6, be provided with in the radio-frequency induction coil 6
Columniform silica crucible 2, the lower end of crucible 2 has the 0.3 ± 0.05mm wide slit injector parallel with running roller 8, vacuum chamber 5 is provided with vavuum pump 11 and external communications; The top board of vacuum chamber 5 is provided with little vacuum chamber 1, and little vacuum chamber 1 has the import of Ar gas, and the bottom of little vacuum chamber 1 is communicated with the upper end open of crucible 2, and the side in vacuum chamber 5 is provided with collecting chamber 3, and the foil of preparing 4 enters in the collecting chamber 3 and collects.The number of turn of radio-frequency induction coil 6 prepares the fusing point of composite insulating foil material and mutual temperature contrast coiling thereof as required.Select the adjustable single-phase asynchronous motor of angular speed 7 for use, can satisfy the preparation needs of different-thickness foil.
The preparation method of high-entropy alloy solder of the present invention uses said apparatus to implement according to following steps,
Steps A, the molten foundry alloy of joining: with high pure metal Ti, Al, Fe, Cu, Ni, Co, Sn, interpolation element (Bi, Ga, In or RE) molten joining in the ultrahigh vacuum electric arc furnaces, the purity of each high pure metal is 99.99%, and concrete steps are:
A1, at first various high pure metals are carried out purified treatment with boric anhydride, again according to good each high pure metal of atomic percent difference weighing: total percentage is 100%, wherein Ti 6%～14%, Al 10%～20%, Fe 10%～20%, Cu 15%～25%, Ni 10%～18%, Co 6%～14%, Sn 0.5%～4.5%, add element 0.03%～3.5%, interpolation element wherein select for use Bi, Ga, In or RE one of them;
A2, the combination that steps A 1 load weighted various high pure metals are added element according to Cu-Sn, Cu-Ni, Ti-Al, Fe-Co-are melted respectively and are joined, and obtain four groups of intermediate alloys;
A3, with the molten four groups of intermediate alloys that prepare of steps A 2, carry out secondary according to Cu-Sn and Cu-Ni, Ti-Al and Fe-Co-interpolation element combinations together and melt and join, obtain two groups of secondary intermediate alloys;
A4, two groups of secondary intermediate alloy Cu-Sn-Ni that again steps A 3 obtained and Ti-Al-Fe-Co-add element and melt and join, and obtain high entropy foundry alloy;
Step B, use above-mentioned single roller quick solidification apparatus and prepare the high-entropy alloy solder foil, the high entropy foundry alloy that steps A 4 obtains is put into crucible 2, open vavuum pump 11, fill high-purity Ar gas to 1.0 ± 0.05KPa after being evacuated to 0.02 ± 0.005Pa; After the process that " vacuumizes-fill Ar gas " repeatedly 3～5 times, opening the high entropy foundry alloy of radio-frequency induction coil 6 heating makes its fusing and crosses thermosetting alloy liquid, after 3～5 minutes, open motor 7 and drive running roller 8 rotation at a high speed, the roll surface speed of running roller 8 is controlled at 5～40m/s, open the Ar air valve immediately, high speed Ar air-flow sprays alloy liquid rapidly, stream is mapped to the roller quench solidification of surperficial also moment of the running roller 8 of rotation at a high speed, the running roller tangential direction throws away in the centrifugal action lower edge, fall into collecting chamber 3 and collect, form the high-entropy alloy solder foil.
High-entropy alloy solder of the present invention is by many pivots of Ti-Al-Fe-Cu-Ni-Co alloy composition, and the high entropy solder foil thickness of making is 25～60 μ m, and wide about 3～7mm is about 1～2m.
During with the assembling of the sample joint of high-entropy alloy solder soldering copper and aluminium, earlier foil is placed between copper material to be welded and the aluminium, according to conventional vacuum brazing method the joint that has assembled is heated, is incubated and solidifies then, realize that copper is connected with the soldering of aluminium.The soldering processes that use high-entropy alloy solder paper tinsel of the present invention to carry out copper and aluminium joint are simple, easy to operate.
Below describe with specific embodiment.
Embodiment 1: according to each component element of the data decimation in the table 1 and control, implements according to following steps,
Steps A, molten join foundry alloy: take by weighing each high pure metal Ti, Al, Fe, Cu, Ni, Co, Sn, interpolation element Bi, and in the ultrahigh vacuum electric arc furnaces molten joining,
A1, at first various high pure metals are carried out purified treatment, again according to good each high pure metal of weighing respectively of the atomic percent in the table 1 with boric anhydride;
A2, with steps A 1 load weighted various high pure metals, the combination of adding element according to Cu-Sn, Cu-Ni, Ti-Al, Fe-Co-is melted respectively and is joined, and obtains four groups of intermediate alloys;
A3, with the molten four groups of intermediate alloys that prepare of steps A 2, carry out secondary according to Cu-Sn and Cu-Ni, Ti-Al and Fe-Co-interpolation element combinations together and melt and join, obtain two groups of secondary intermediate alloys;
A4, two groups of secondary intermediate alloy Cu-Sn-Ni that again steps A 3 obtained and Ti-Al-Fe-Co-add element and melt and join, and obtain high entropy foundry alloy;
Step B, the single roller quick solidification apparatus of application prepare the high-entropy alloy solder foil, and the high entropy foundry alloy that steps A 4 obtains is put into
Cylindrical crucible in, crucible bottom has the wide slit injector of 0.3mm, crucible is held in place in the radio-frequency induction coil at running roller top again, opens vavuum pump, fills high-purity Ar gas to 1.0 ± 0.05KPa after being evacuated to 0.02 ± 0.005Pa; After the process that " vacuumizes-fill Ar gas " repeatedly 3 times, using high-frequency induction equipment to heat high entropy foundry alloy makes its fusing and crosses thermosetting alloy liquid, after 5 minutes, open motor, running roller rotates at a high speed, and roll surface speed is controlled at 5m/s, open the Ar air valve immediately, high speed Ar air-flow sprays alloy liquid rapidly, stream be mapped at a high speed rotation the running roller surface and moment quench solidification, throw away and form the high-entropy alloy solder foil in centrifugal action lower edge running roller tangential direction.
Prepare the amorphous state high-entropy alloy solder foil of thick about 55 μ m, use this high-entropy alloy solder foil, T
2Fine copper and 6061 aluminium alloys weld, and joint draws cuts the about 131.2MPa of intensity, reach 6061 aluminium alloys name intensity (σ
b=180MPa) 73%.
Embodiment 2: according to the step of the foregoing description 1, according to each component element of the data decimation in the table 1 and content, roll surface speed is controlled at 10m/s, can prepares the amorphous state high-entropy alloy solder foil of thick about 50 μ m.Use this high-entropy alloy solder foil, to T
2Fine copper and 6061 aluminium alloys weld, and joint draws cuts the about 139.5MPa of intensity, reach 6061 aluminium alloys name intensity (σ
b=180MPa) 77.5%.
Table 1 is the tables of data of each embodiment
| Constituent content and control parameter | Ti 6-14 | Al 10-20 | Fe 10-20 | Cu 15-25 | Ni 10-18 | Co 6-14 | Sn 0.5-4.5 | Add element 0.03-3.5 |
| Embodiment 1 | 13 | 17 | 20 | 25 | 10 | 14 | 0.97 | Getting Bi is 0.03 |
| |
13 | 20 | 20 | 15 | 17 | 13.4 | 1.5 | Getting Ga is 0.1 |
| |
6 | 20 | 17 | 24 | 18 | 11 | 2.5 | Getting In is 1.5 |
| |
14 | 10 | 20 | 20 | 15 | 13 | 4.5 | Getting RE is 3.5 |
| |
14 | 20 | 15 | 25 | 18 | 6 | 1 | Getting RE is 1 |
| |
14 | 20 | 20 | 15 | 17 | 11 | 0.5 | Getting In is 2.5 |
| |
12 | 20 | 10 | 25 | 18 | 12 | 1 | Getting Ga is 2 |
| |
13 | 20 | 18 | 22 | 10 | 14 | 2.94 | Getting Bi is 0.06 |
Embodiment 3: according to the step of the foregoing description 1, according to each component element of the data decimation in the table 1 and content, roll surface speed is controlled at 15m/s, can prepares the amorphous state high-entropy alloy solder foil of thick about 45 μ m.Use this high-entropy alloy solder foil, to T
2Fine copper and 6061 aluminium alloys weld, and joint draws cuts the about 135.3MPa of intensity, reach 6061 aluminium alloys name intensity (σ
b=180MPa) 75.2%.
Embodiment 4: according to the step of the foregoing description 1, according to each component element of the data decimation in the table 1 and content, roll surface speed is controlled at 20m/s, can prepares the amorphous state high-entropy alloy solder foil of thick about 45 μ m.Use this high-entropy alloy solder foil, to T
2Fine copper and 6061 aluminium alloys weld, and joint draws cuts the about 129.8MPa of intensity, reach 6061 aluminium alloys name intensity (σ
b=180MPa) 72.1%.
Embodiment 5: according to the step of the foregoing description 1, according to each component element of the data decimation in the table 1 and content, roll surface speed is controlled at 25m/s, can prepares the amorphous state high-entropy alloy solder foil of thick about 40 μ m.Use this high-entropy alloy solder foil, to T
2Fine copper and 6061 aluminium alloys weld, and joint draws cuts the about 130.2MPa of intensity, reach 6061 aluminium alloys name intensity (σ
b=180MPa) 72.99%.
Embodiment 6: according to the step of the foregoing description 1, according to each component element of the data decimation in the table 1 and content, roll surface speed is controlled at 30m/s, can prepares the amorphous state high-entropy alloy solder foil of thick about 35 μ m.Use this high-entropy alloy solder foil, to T
2Fine copper and 6061 aluminium alloys weld, and joint draws cuts the about 139.8MPa of intensity, reach 6061 aluminium alloys name intensity (σ
b=180MPa) 77.52%.
Embodiment 7: according to the step of the foregoing description 1, according to each component element of the data decimation in the table 1 and content, roll surface speed is controlled at 35m/s, can prepares the amorphous state high-entropy alloy solder foil of thick about 30 μ m.Use this high-entropy alloy solder foil, to T
2Fine copper and 6061 aluminium alloys weld, and joint draws cuts the about 134.3MPa of intensity, reach 6061 aluminium alloys name intensity (σ
b=180MPa) 75.1%.
Embodiment 8: according to the step of the foregoing description 1, according to each component element of the data decimation in the table 1 and content, roll surface speed is controlled at 40m/s, can prepares the amorphous state high-entropy alloy solder foil of thick about 25 μ m.Use this high-entropy alloy solder foil, to T
2Fine copper and 6061 aluminium alloys weld, and joint draws cuts the about 129.9MPa of intensity, reach 6061 aluminium alloys name intensity (σ
b=180MPa) 72.15%.
In sum, high-entropy alloy solder of the present invention, the solder flexility is good, is convenient to processing and assembling; When welding with Al, Cu metal matching is good, the brazed seam decay resistance is good, weld seam is single-phase fcc solid solution tissue, compound generation between no brittle metal, the joint comprehensive mechanical performance significantly improves; The preparation method of this kind high-entropy alloy solder, technology is simple, and cost of manufacture is low, is convenient to promote.
Claims (2)
1, a kind of high-entropy alloy solder that is used for soldering copper and aluminium is characterized in that: be made up of by atomic percent following component:
Total percentage is 100%, wherein Ti 6%～14%, Al 10%～20%, Fe 10%～20%, Cu 15%～25%, Ni 10%～18%, Co 6%～14%, Sn 0.5%～4.5%, add element 0.03%～3.5%, interpolation element wherein select for use Bi, Ga, In or RE one of them.
2, the preparation method of the described high-entropy alloy solder of a kind of claim 1, it is characterized in that: this method is implemented according to following steps,
Steps A, the molten foundry alloy of joining: with high pure metal Ti, Al, Fe, Cu, Ni, Co, Sn, interpolation element molten joining in the ultrahigh vacuum electric arc furnaces, concrete steps are:
A1, at first various high pure metals are carried out purified treatment with boric anhydride, again according to the good various high pure metals of atomic percent difference weighing: total percentage is 100%, wherein Ti 6%～14%, Al 10%～20%, Fe 10%～20%, Cu 15%～25%, Ni 10%～18%, Co 6%～14%, Sn 0.5%～4.5%, add element 0.03%～3.5%, interpolation element wherein select for use Bi, Ga, In or RE one of them;
A2, with steps A 1 load weighted various high pure metals, the combination of adding element according to Cu-Sn, Cu-Ni, Ti-Al, Fe-Co-is melted respectively and is joined, and obtains four groups of intermediate alloys;
A3, with the molten four groups of intermediate alloys that prepare of steps A 2, add element combinations according to Cu-Sn and Cu-Ni, Ti-Al and Fe-Co-and carry out secondary together and melt and join, obtain two groups of secondary intermediate alloy Cu-Sn-Ni and Ti-Al-Fe-Co-interpolation element;
A4, two groups of secondary intermediate alloy Cu-Sn-Ni that again steps A 3 obtained and Ti-Al-Fe-Co-add element and melt and join, and obtain high entropy foundry alloy;
Step B, use single roller quick solidification apparatus and prepare high-entropy alloy solder, the molten high entropy foundry alloy for preparing of steps A is put into crucible, crucible bottom has slit injector, after the process that " vacuumizes-fill Ar gas " repeatedly 3～5 times, using high-frequency induction equipment to heat high entropy foundry alloy makes its fusing and crosses thermosetting alloy liquid, after 3～5 minutes, open the rotation of driven by motor running roller, roll surface speed is controlled at 5～40m/s, open the Ar air valve immediately, high speed Ar air-flow sprays alloy liquid rapidly, and stream is mapped to the running roller quench solidification of surperficial also moment of rotation at a high speed, throw away along the running roller tangential direction, obtain the high-entropy alloy solder foil.
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