CN109465563B - Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy solder and preparation method thereof - Google Patents
Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy solder and preparation method thereof Download PDFInfo
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- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 80
- 239000000956 alloy Substances 0.000 title claims abstract description 80
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 74
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910000679 solder Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000005219 brazing Methods 0.000 claims abstract description 95
- 229910052751 metal Inorganic materials 0.000 claims abstract description 73
- 239000002184 metal Substances 0.000 claims abstract description 73
- 239000000945 filler Substances 0.000 claims abstract description 64
- 238000005266 casting Methods 0.000 claims abstract description 45
- 238000005097 cold rolling Methods 0.000 claims abstract description 31
- 238000005096 rolling process Methods 0.000 claims abstract description 30
- 238000009750 centrifugal casting Methods 0.000 claims abstract description 27
- 239000010949 copper Substances 0.000 claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 54
- 238000010438 heat treatment Methods 0.000 claims description 50
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 32
- 229910002804 graphite Inorganic materials 0.000 claims description 32
- 239000010439 graphite Substances 0.000 claims description 32
- 229910052759 nickel Inorganic materials 0.000 claims description 24
- 229910052802 copper Inorganic materials 0.000 claims description 22
- 239000011777 magnesium Substances 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 21
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- 230000006698 induction Effects 0.000 claims description 19
- 239000010936 titanium Substances 0.000 claims description 19
- 229910052749 magnesium Inorganic materials 0.000 claims description 17
- 229910052797 bismuth Inorganic materials 0.000 claims description 16
- 238000002844 melting Methods 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 15
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 14
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 12
- 238000012545 processing Methods 0.000 claims description 12
- 238000007670 refining Methods 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 11
- 229910052710 silicon Inorganic materials 0.000 claims description 11
- 229910018125 Al-Si Inorganic materials 0.000 claims description 10
- 229910018182 Al—Cu Inorganic materials 0.000 claims description 10
- 229910018520 Al—Si Inorganic materials 0.000 claims description 10
- 229910018575 Al—Ti Inorganic materials 0.000 claims description 10
- 238000000137 annealing Methods 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 238000003825 pressing Methods 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- VHHHONWQHHHLTI-UHFFFAOYSA-N hexachloroethane Chemical compound ClC(Cl)(Cl)C(Cl)(Cl)Cl VHHHONWQHHHLTI-UHFFFAOYSA-N 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 238000007872 degassing Methods 0.000 claims description 6
- 238000010791 quenching Methods 0.000 claims description 6
- 230000000171 quenching effect Effects 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 5
- 150000002739 metals Chemical class 0.000 claims description 5
- 229910052700 potassium Inorganic materials 0.000 claims description 5
- 239000011591 potassium Substances 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 5
- JRBRVDCKNXZZGH-UHFFFAOYSA-N alumane;copper Chemical compound [AlH3].[Cu] JRBRVDCKNXZZGH-UHFFFAOYSA-N 0.000 claims description 4
- 229910021420 polycrystalline silicon Inorganic materials 0.000 claims description 4
- 229910001094 6061 aluminium alloy Inorganic materials 0.000 claims description 2
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- 229910000838 Al alloy Inorganic materials 0.000 abstract description 20
- WPPDFTBPZNZZRP-UHFFFAOYSA-N aluminum copper Chemical compound [Al].[Cu] WPPDFTBPZNZZRP-UHFFFAOYSA-N 0.000 abstract description 7
- 230000009286 beneficial effect Effects 0.000 abstract description 3
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- 229910000831 Steel Inorganic materials 0.000 description 11
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- 239000011888 foil Substances 0.000 description 8
- 229910000765 intermetallic Inorganic materials 0.000 description 7
- 229910018565 CuAl Inorganic materials 0.000 description 5
- 239000010953 base metal Substances 0.000 description 4
- 239000004927 clay Substances 0.000 description 4
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- 229910017944 Ag—Cu Inorganic materials 0.000 description 1
- 229910017942 Ag—Ge Inorganic materials 0.000 description 1
- 229910018566 Al—Si—Mg Inorganic materials 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229910018594 Si-Cu Inorganic materials 0.000 description 1
- 229910008465 Si—Cu Inorganic materials 0.000 description 1
- 229910008310 Si—Ge Inorganic materials 0.000 description 1
- 229910006776 Si—Zn Inorganic materials 0.000 description 1
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/28—Selection of soldering or welding materials proper with the principal constituent melting at less than 950 degrees C
- B23K35/286—Al as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
- B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
- B23K35/0233—Sheets, foils
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
Abstract
An Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy solder and a preparation method thereof, the solder comprises the following components by weight: 15-25 wt% of Cu, 5-7 wt% of Si, 1-5 wt% of Ni, 0.3-1.0 wt% of Mg, 0.05-0.2 wt% of Ti, 0.1-0.3 wt% of Bi and the balance of Al. The preparation method adopts the steps of casting, centrifugal casting, superplastic treatment, isothermal rolling and cold rolling, and is simple and beneficial to batch production. The method can be used for preparing the foil-shaped brazing filler metal with the thickness of 0.03mm, and is suitable for the requirements of vacuum brazing of various aluminum alloy components and vacuum brazing of aluminum-copper heterogeneous metal components.
Description
Technical Field
The invention relates to an Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy foil-shaped brazing filler metal and a preparation method thereof, which are mainly used for vacuum brazing of aluminum-copper heterogeneous metal, can also be matched with an aluminum-based medium-temperature brazing filler metal to realize aluminum alloy graded brazing, and simultaneously fill the defect of poor wettability of the aluminum-based low-temperature brazing filler metal, and belong to the technical field of metallurgy and calendaring processing.
Background
Brazing means that metal with liquidus temperature lower than that of a base metal is used as brazing filler metal, parts and the brazing filler metal are heated until the brazing filler metal is molten, the base metal is wetted by the brazing filler metal, a joint gap is filled, and the brazing filler metal and the base metal are mutually dissolved and diffused to realize the method for connecting the parts. The copper-aluminum dissimilar metal joint has excellent mechanical property, electric conductivity and heat conductivity, and can be applied to various industrial fields, such as electrical engineering, chemical engineering and refrigeration industry. The aluminum-copper joint can adopt the forms of pressure welding, fusion welding, brazing and diffusion welding, wherein the brazing has the characteristics of low heating temperature, small influence on the structure and the performance of a base material, high precision and the like, and is a main method for aluminum-copper connection. The vacuum brazing does not need brazing flux, can reduce the corrosion to the base metal, and is suitable for processing high-performance aluminum-copper joints.
Aluminum alloy vacuum brazing generally adopts Al-Si-Mg brazing filler metal, particularly 4004 components, but the melting temperature is higher. Known aluminum alloy medium temperature brazing filler metal grades such as Al-Si-Cu, Al-Si-Ge, Al-Si-Zn, Al-Ag-Ge, Al-Ag-Cu and the like are very brittle, are only suitable for casting strips and are difficult to process into foil-shaped brazing filler metal, and have poor corrosion resistance and brazing manufacturability. Brazing of aluminum alloy and copper requires a brazing temperature of no more than 545 ℃ to reduce the CuAl2The content of intermetallic compounds and the thickness of the copper-aluminum reaction layer so as to ensure the strength and the corrosion resistance of the joint. Therefore, the brazing filler metal with the melting temperature of 450-520 ℃ is urgently needed to be developed, and the bottleneck of vacuum brazing of aluminum alloy and copper is solved.
Disclosure of Invention
The invention aims to provide an Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy foil-shaped brazing filler metal and a preparation method thereof, wherein the brazing filler metal has low melting temperature: the brazing filler metal is 495-515 ℃, has thin thickness (about 0.03 mm), has good wettability and mechanical property, can realize vacuum brazing at the temperature of not higher than 540 ℃, is suitable for low-temperature or graded vacuum brazing of various aluminum alloys such as 3A21, 2A50, 6063 and 6061, and can also be used for vacuum brazing of aluminum-copper heterogeneous metals.
In order to achieve the purpose, the invention adopts the following technical scheme:
an Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy solder comprises the following components in percentage by weight: 15-25 wt% of Cu, 5-7 wt% of Si, 1-5 wt% of Ni, 0.3-1.0 wt% of Mg, 0.05-0.2 wt% of Ti, 0.1-0.3 wt% of Bi and the balance of Al.
The Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy solder as described above preferably has a composition of: 18 to 22 wt% of Cu, 5 to 7 wt% of Si, 1.5 to 2.5 wt% of Ni, 0.3 to 1 wt% of Mg, 0.1 to 0.2 wt% of Ti, 0.2 to 0.3 wt% of Bi, and the balance of Al.
The Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy solder is preferably foil-shaped, and the thickness of the solder is 0.03-0.15 mm.
On the other hand, the invention provides a preparation method of Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy brazing filler metal, which adopts the steps of casting, centrifugal casting, superplastic treatment, isothermal rolling and cold rolling and specifically comprises the following steps:
I. preparing materials: the purity of aluminum is more than 99.9 percent, the purity of copper is oxygen-free copper, the purity of silicon is more than 99.99 percent, the purity of nickel is more than 99.9 percent, the purity of magnesium is more than 99.99 percent, the purity of titanium is more than 99.99 percent, and the purity of bismuth is more than 99.99 percent; weighing the raw materials according to the mass percentage of the components;
II, preparing an intermediate alloy:
(I) adding an aluminum ingot into a graphite crucible of a medium-frequency induction furnace, heating to melt the aluminum ingot, adding a copper ingot, heating the furnace to 750-800 ℃, fully stirring, casting a ingot after the copper ingot is completely melted, and casting the ingot at an alloy casting temperature of 700-750 ℃ to obtain an Al-Cu intermediate alloy;
(II) adding an aluminum ingot into a graphite crucible of the medium-frequency induction furnace, heating the graphite crucible to 800-850 ℃ after the aluminum ingot is melted, pressing polycrystalline silicon into aluminum liquid, keeping the temperature at 800-850 ℃ for 10-15 min after the polycrystalline silicon is completely melted down, fully stirring, casting ingots, and casting the alloys at the temperature of 850-900 ℃ to obtain Al-Si intermediate alloys;
(III) adding an aluminum ingot into a graphite crucible of a medium-frequency induction furnace, heating the graphite crucible to 1000-1050 ℃ after the aluminum ingot is melted, adding pure titanium, keeping the temperature at 1000-1050 ℃ for 10-15 min after the titanium is completely melted, fully stirring, casting ingots, and casting the alloys at 1050-1100 ℃ to obtain Al-Ti intermediate alloys;
and III, alloy casting: putting pure aluminum into a graphite crucible of a medium-frequency induction furnace, heating, sequentially adding Al-Cu, Al-Si, Al-Ti intermediate alloy and a pure nickel belt after aluminum ingots are completely melted, heating to 750-800 ℃ after the intermediate alloy and the nickel are completely melted, preserving heat for 10-15 min, pressing hexachloroethane into the bottom of alloy liquid by using a graphite cover, stirring, degassing, slagging, scattering a little refining agent which selects potassium fluoroaluminate, removing surface scum, heating to 650-700 ℃, adding magnesium and bismuth, fully stirring, and casting to obtain cast ingots;
IV, centrifugal casting: crushing the cast brazing filler metal ingot, putting the crushed cast brazing filler metal ingot into a graphite crucible in a centrifugal casting furnace, melting the crushed cast brazing filler metal ingot under the protection of Ar gas, heating the ingot to 650-700 ℃ after the ingot is completely melted, and casting the ingot into a sheet with the thickness of 1.5-2.5 mm by adopting a centrifugal casting mode;
v, superplasticizing treatment: placing the sheet obtained in the step IV into a resistance furnace, preserving heat for 12-16 hours at 400-420 ℃, then heating to 480-490 ℃, preserving heat for 30-45 min, and quenching;
VI, isothermal rolling: c, heating the plate blank obtained in the step V at the temperature of 450-460 ℃, rolling the plate blank at the temperature of 450-460 ℃ by a rolling mill, and carrying out isothermal rolling with the pass processing rate of 3-5% to obtain a strip with the thickness of 0.5-0.7 mm;
VII, cold rolling: cold rolling the strip subjected to isothermal rolling at the temperature of 5-50 ℃, and then annealing at the temperature of 420-450 ℃ for 1.5-2 h; and (4) cold rolling in multiple times until the required thickness is obtained.
In the preparation method as described above, preferably, in the step II, the content of copper in the Al-Cu master alloy is 50 wt%, the content of silicon in the Al-Si master alloy is 30 wt%, and the content of titanium in the Al-Ti master alloy is 5 wt%.
In the preparation method, preferably, the hexachloroethane is used in an amount of 0.3-0.4 wt% of the furnace amount in the step III, and the refining agent is used in an amount of 0.2-0.3 wt% of the furnace amount.
In the preparation method, preferably, in the step VII, the cold rolling pass reduction is controlled to be 3% to 5%, and the total cold rolling reduction is 9% to 15%.
In still another aspect, the present invention provides an Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy solder prepared by the method as described above.
In a further aspect, the present invention provides the use of an Al-Cu-Si-Ni-Mg-Ti-Bi aluminium based alloyed solder as described above in low temperature or staged vacuum brazing of 3A21, 2A50, 6063 and 6061 aluminium alloys, and in vacuum brazing of aluminium-copper dissimilar metals.
The brazing filler metal of the invention is medium-temperature seven-component brazing filler metal based on AlCuSi ternary eutectic system. Wherein, one function of adding Mg element is to reduce melting point, and the other function is to destroy the oxide film of the substrate in vacuum brazing, so that the dissolution and diffusion between the brazing filler metal and the substrate occur. One function of the Ni addition is to change the CuAl in the solder2The shape of the intermetallic compound reduces the brittleness of the brazing filler metal and improves the processing performance of the brazing filler metal; another effect is to improve the corrosion resistance of the joint. Bi is added to promote the wettability of the brazing filler metal and the aluminum alloy base material and improve the brazing performance. Ti element is added to weaken the action of brazing filler metal and copper base material, reduce the thickness of a reaction layer, reduce the brittleness of the joint and improve the strength of the joint. The brazing filler metal has scientific component design and reasonable proportion, and can be popularized and applied to brazing of various aluminum alloy components. The beneficial effects of the invention are as follows:
(1) the Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy foil solder is suitable for vacuum brazing of various aluminum alloys such as 3A21, 2A50, 6063 and 6061, and the like, and can also be used for vacuum brazing of aluminum alloy and copper dissimilar metal; the thickness of the brazing filler metal can reach 0.03mm, and the brazing filler metal is suitable for vacuum brazing of various aluminum alloy components and aluminum-copper heterogeneous metal components.
(2) The Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy foil solder has low melting temperature of 495-515 ℃, and can complete vacuum brazing on aluminum alloy at the temperature of not higher than 540 ℃; the brazing filler metal has good brazing manufacturability and good wettability, and the welding rate is higher than 95%; tensile strength of weldbNot less than 90MPa, and the shearing strength tau not less than 60 MPa.
(3) The method for preparing the Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy foil-shaped brazing filler metal combines casting, centrifugal casting, superplastic treatment, isothermal rolling and cold rolling processes, and the thickness of the prepared foil-shaped brazing filler metal reaches 0.03 mm. Wherein, firstly, a thin plate with the thickness of 1-2mm is prepared by centrifugal casting; the superplastic treatment step refines alloy grains to make the alloy components uniform; the isothermal rolling step enables the alloy to be changed from a casting state to a rolling state, has cold processing performance, and further reduces the thickness of the brazing filler metal to 0.8mm per month; finally, multi-pass cold rolling is adopted to obtain the foil-shaped brazing filler metal with the required thickness, and the obtained brazing filler metal is smooth in surface and uniform in thickness. The method is simple and is beneficial to large-scale batch production.
Drawings
FIG. 1 is a differential thermal analysis spectrum of an Al-Cu-Si-Ni-Mg-Ti-Bi alloy-state foil solder obtained in example 1 of the present invention.
FIG. 2 is a metallographic photograph showing an as-cast structure of an Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy brazing filler metal prepared in comparative example 1 of the present invention.
FIG. 3 is a metallographic photograph showing an as-cast structure of an Al-Cu-Si-Mg-Ti-Bi aluminum-based alloy brazing filler metal prepared in comparative example 1 of the present invention.
Detailed Description
The Al-Cu-Si-Ni-Mg-Ti-Bi alloy-state foil solder and the preparation method thereof according to the present invention will be further described below with reference to examples of specific compounding calculations.
The materials selected and master alloys of the following examples were prepared as follows:
aluminum: selecting high-purity aluminum with the purity of more than 99.9 percent; the copper is oxygen-free copper; the purity of the selected silicon is more than 99.99 percent; the purity of the selected nickel is more than 99.9 percent; the purity of magnesium should be more than 99.99%, the purity of titanium should be more than 99.99%, and the purity of bismuth should be more than 99.99%.
Preparing an intermediate alloy:
melting of Al-Cu50 intermediate alloy
1) Equipment: 10kg of intermediate frequency induction furnace;
2) a mould: water-cooling the steel die: 30X 210X 440 mm;
3) preparing materials: 10kg of materials are mixed in each furnace;
4) the operation is as follows: and adding an aluminum ingot into the graphite clay crucible, heating, adding a copper ingot after the aluminum ingot is melted, heating the furnace to 700-750 ℃, fully stirring, and casting ingots at the alloy casting temperature of 700-750 ℃ after the copper ingot is completely melted.
Melting of Al-Si30 intermediate alloy
1) Equipment: 10kg of intermediate frequency induction furnace;
2) a mould: water-cooling the steel die: 30X 210X 440 mm;
3) preparing materials: 10kg of materials are mixed in each furnace;
4) the operation is as follows: adding an aluminum ingot into a graphite clay crucible, heating the furnace to 800 ℃ after the aluminum ingot is melted, pressing silicon into the aluminum liquid, keeping the temperature at 800 ℃ for 10min after the silicon is completely melted down, fully stirring, and casting ingots at the alloy casting temperature of 850-900 ℃.
Melting of Al-Ti5 intermediate alloy
1) Equipment: 10kg of intermediate frequency induction furnace;
2) a mould: water-cooling the steel die: 30X 210X 440 mm;
3) preparing materials: 10kg of materials are mixed in each furnace;
4) the operation is as follows: adding an aluminum ingot into a graphite clay crucible, heating the graphite clay crucible until the aluminum ingot is molten, heating the furnace to 1000 ℃, adding pure titanium, keeping the temperature at 1000 ℃ for 10min after the titanium is completely molten, fully stirring, and casting ingots at the alloy casting temperature of 1050-1100 ℃.
EXAMPLE 1 preparation of Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy foil-shaped brazing filler Metal (I)
Step 1: ingredients
Al-Cu5022kg, Al-Si3010kg, Al-Ti51kg, 15.25kg of aluminum, 1.25kg of nickel, 0.4kg of magnesium and 0.1kg of bismuth are taken.
Step 2: alloy casting
1) Equipment: 150kg of medium frequency induction furnace;
2) a mould: a phi 80 multiplied by 300mm water-cooled steel die;
3) preparing materials: the added return material does not exceed 30% of the furnace amount;
4) the operation is as follows: putting pure aluminum into a graphite crucible of a medium-frequency induction furnace, heating, adding Al-Cu, Al-Si, Al-Ti intermediate alloy and a pure nickel belt in sequence after aluminum ingots are completely melted, heating to 750 ℃ after the intermediate alloy and the nickel are completely melted, preserving heat for 15min, pressing hexachloroethane into the bottom of alloy liquid by a graphite cover, stirring, degassing, slagging, scattering a little refining agent after slagging is finished, removing surface scum by the refining agent, heating to 650 ℃, adding magnesium and bismuth, fully stirring, and casting to obtain cast ingots.
And step 3: centrifugal casting
1) Equipment: a centrifugal casting furnace;
2) a mould: a water-cooled steel die with the thickness of 10 multiplied by 200 multiplied by 300 mm;
and crushing the cast brazing filler metal ingot, putting the crushed ingot into a graphite crucible in a centrifugal casting furnace, melting the crushed ingot under the protection of Ar gas, heating the melted ingot to 650 ℃ after the melted ingot is completely melted, and casting the melted ingot into a thin plate with the thickness of 2mm by adopting a centrifugal casting mode.
And 4, step 4: ultra-plasticizing treatment
1) Equipment: a resistance furnace;
2) the operation is as follows: and placing the obtained cast ingot in a resistance furnace, preserving heat for 12 hours at 400, then heating to 480, preserving heat for 30min, and quenching.
And 5: isothermal rolling
The heating temperature of the plate blank is 450-460 ℃, the rolling temperature of the rolling mill is 450-460 ℃, the pass processing rate is 3-5%, and the thin plate with the thickness of 0.55mm is manufactured.
Step 6: cold rolling
The cold rolling pass working ratio is controlled to be 3% -5%, annealing treatment is carried out after cold rolling, the annealing temperature is 460 ℃, and heat preservation is carried out for 2 hours to eliminate work hardening. The total working rate of the third cold rolling is 12 percent, and the foil-shaped aluminum alloy brazing filler metal with the thickness of 0.03mm is obtained, and contains 22wt percent of Cu, 6wt percent of Si, 2.5wt percent of Ni, 0.8wt percent of Mg, 0.1wt percent of Ti, 0.2wt percent of Bi and the balance of aluminum.
The differential thermal analysis curve of the prepared foil-shaped brazing filler metal is shown in the attached figure 1 of the specification, wherein Te is the solidus temperature of the brazing filler metal alloy 496 ℃, and Tf is the liquidus temperature of the brazing filler metal alloy 515 ℃.
EXAMPLE 2 preparation of Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy foil solder (II)
Step 1: ingredients
Taking Al-Cu5028.5kg, Al-Si3017.5kg, Al-Ti50.75kg, aluminum 26.6kg, nickel 0.75kg, magnesium 0.75kg and bismuth 0.15 kg.
Step 2: alloy casting
1) Equipment: 150kg of medium frequency induction furnace;
2) a mould: a phi 80 multiplied by 300mm water-cooled steel die;
3) preparing materials: the added return material does not exceed 30% of the furnace amount;
4) the operation is as follows: putting pure aluminum into a graphite crucible of a medium-frequency induction furnace, heating, adding Al-Cu, Al-Si, Al-Ti intermediate alloy and a pure nickel belt in sequence after aluminum ingots are completely melted, heating to 780 ℃ after the intermediate alloy and the nickel are completely melted, preserving heat for 12min, pressing hexachloroethane into the bottom of alloy liquid by a graphite cover, stirring, degassing, slagging, spreading a little refining agent, selecting potassium fluoroaluminate as the refining agent, removing surface scum, heating to 680 ℃, adding magnesium and bismuth, fully stirring, and casting to obtain cast ingots.
And step 3: centrifugal casting
1) Equipment: a centrifugal casting furnace;
2) a mould: a water-cooled steel die with the thickness of 10 multiplied by 200 multiplied by 300 mm;
and crushing the cast brazing filler metal ingot, putting the crushed ingot into a graphite crucible in a centrifugal casting furnace, melting the crushed ingot under the protection of Ar gas, heating the melted ingot to 660 ℃ after the melted ingot is completely melted, and casting the melted ingot into a thin plate with the thickness of 2.5mm by adopting a centrifugal casting mode.
And 4, step 4: ultra-plasticizing treatment
1) Equipment: a resistance furnace;
2) the operation is as follows: and placing the obtained cast ingot in a resistance furnace, preserving heat for 12 hours at 420 ℃, then heating to 485 ℃, preserving heat for 30min, and quenching.
And 5: isothermal rolling
The heating temperature of the plate blank is 450-460 ℃, the rolling temperature of the rolling mill is 450-460 ℃, the pass processing rate is 3-5%, and the thin plate with the thickness of 0.6mm is manufactured.
Step 6: cold rolling
The cold rolling pass reduction rate is controlled to be 3% -5%, annealing treatment is carried out after cold rolling, the annealing temperature is 440 ℃, and heat preservation is carried out for 2 hours to eliminate work hardening. The total working ratio of the third cold rolling is 15, and the foil-shaped aluminum alloy brazing filler metal with the thickness of 0.05mm is obtained, and contains 19 wt% of Cu, 7 wt% of Si, 1 wt% of Ni, 1 wt% of Mg, 0.05 wt% of Ti, 0.2 wt% of Bi and the balance of aluminum.
EXAMPLE 3 preparation of Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy-based foil solder (III)
Step 1: ingredients
Al-Cu5040kg, Al-Si3018.33kg, Al-Ti53kg, aluminum 36.02kg, nickel 2kg, magnesium 0.5kg and bismuth 0.15 kg.
Step 2: alloy casting
1) Equipment: 150kg of medium frequency induction furnace;
2) a mould: a phi 80 multiplied by 300mm water-cooled steel die;
3) preparing materials: the added return material does not exceed 30% of the furnace amount;
4) the operation is as follows: putting pure aluminum into a graphite crucible of a medium-frequency induction furnace, heating, adding Al-Cu, Al-Si, Al-Ti intermediate alloy and a pure nickel belt in sequence after aluminum ingots are completely melted, heating to 800 ℃ after the intermediate alloy and the nickel are completely melted, preserving heat for 10min, pressing hexachloroethane into the bottom of alloy liquid by a graphite cover, stirring, degassing, slagging, spreading a little refining agent, selecting potassium fluoroaluminate as the refining agent, removing surface scum, heating to 670 ℃, adding magnesium and bismuth, fully stirring, and casting to obtain cast ingots.
And step 3: centrifugal casting
1) Equipment: a centrifugal casting furnace;
2) a mould: a water-cooled steel die with the thickness of 10 multiplied by 200 multiplied by 300 mm;
and crushing the cast brazing filler metal ingot, putting the crushed ingot into a graphite crucible in a centrifugal casting furnace, melting the crushed ingot under the protection of Ar gas, heating the melted ingot to 700 ℃ after the melted ingot is completely melted, and casting the melted ingot into a thin plate with the thickness of 1.5mm by adopting a centrifugal casting mode.
And 4, step 4: ultra-plasticizing treatment
1) Equipment: a resistance furnace;
2) the operation is as follows: and placing the obtained cast ingot in a resistance furnace, preserving heat for 12 hours at 400, then heating to 480, preserving heat for 30min, and quenching.
And 5: isothermal rolling
The heating temperature of the plate blank is 450-460 ℃, the rolling temperature of the rolling mill is 450-460 ℃, the pass processing rate is 3-5%, and the thin plate with the thickness of 0.5mm is manufactured.
Step 6: cold rolling
The cold rolling pass working ratio is controlled to be 3% -5%, annealing treatment is carried out after cold rolling, the annealing temperature is 450 ℃, and heat preservation is carried out for 1.5 hours to eliminate work hardening. The total working rate of the third cold rolling is 10 percent, and the foil-shaped aluminum alloy solder with the thickness of 0.08mm is obtained, and contains 20 weight percent of Cu, 5.5 weight percent of Si, 2 weight percent of Ni, 0.5 weight percent of Mg, 0.15 weight percent of Ti, 0.15 weight percent of Bi and the balance of aluminum.
EXAMPLE 4 preparation of Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy foil-shaped brazing filler metal (IV)
Step 1: ingredients
Al-Cu5048kg, Al-Si3020kg, Al-Ti54kg, 23.15kg of aluminum, 4kg of nickel, 0.75kg of magnesium and 0.1kg of bismuth are taken.
Step 2: alloy casting
1) Equipment: 150kg of medium frequency induction furnace;
2) a mould: a phi 80 multiplied by 300mm water-cooled steel die;
3) preparing materials: the added return material does not exceed 30% of the furnace amount;
4) the operation is as follows: putting pure aluminum into a graphite crucible of a medium-frequency induction furnace, heating, adding Al-Cu, Al-Si, Al-Ti intermediate alloy and a pure nickel belt in sequence after an aluminum ingot is completely melted, heating to 775 ℃ after the intermediate alloy and the nickel are completely melted, keeping the temperature for 12min, pressing hexachloroethane into the bottom of alloy liquid by a graphite cover, stirring, degassing and slagging, spreading a little refining agent after slagging is finished, selecting potassium fluoroaluminate as the refining agent, removing surface scum, heating to 675 ℃, adding magnesium and bismuth, fully stirring, and casting to obtain an ingot.
And step 3: centrifugal casting
1) Equipment: a centrifugal casting furnace;
2) a mould: a water-cooled steel die with the thickness of 10 multiplied by 200 multiplied by 300 mm;
and crushing the cast brazing filler metal ingot, putting the crushed ingot into a graphite crucible in a centrifugal casting furnace, melting the crushed ingot under the protection of Ar gas, heating the melted ingot to 675 ℃ after complete melting, and casting the melted ingot into a thin plate with the thickness of 2.25mm by adopting a centrifugal casting mode.
And 4, step 4: ultra-plasticizing treatment
1) Equipment: a resistance furnace;
2) the operation is as follows: and placing the obtained cast ingot in a resistance furnace, preserving heat for 12 hours at 415 ℃, then heating to 485 ℃, preserving heat for 30min, and quenching.
And 5: isothermal rolling
The heating temperature of the plate blank is 450-460 ℃, the rolling temperature of the rolling mill is 450-460 ℃, the pass processing rate is 3-5%, and the thin plate with the thickness of 0.65mm is manufactured.
Step 6: cold rolling
The cold rolling pass working ratio is controlled to be 3% -5%, annealing treatment is carried out after cold rolling, the annealing temperature is 425 ℃, and heat preservation is carried out for 2 hours to eliminate work hardening. The total working rate of the third cold rolling is 12 percent, and the foil-shaped aluminum alloy brazing filler metal with the thickness of 0.10mm is obtained, and contains 24 weight percent of Cu, 6 weight percent of Si, 4 weight percent of Ni, 0.75 weight percent of Mg, 0.2 weight percent of Ti, 0.1 weight percent of Bi and the balance of aluminum.
Example 5 Performance test
The foil-shaped brazing filler metals prepared in example 1, example 2, example 3 and example 4 were used for physical tests and vacuum brazing tests of aluminum alloys, respectively, and the test data were obtained as shown in table 1.
TABLE 1
Comparative example 1
(one) an aluminum alloy ingot was obtained by the same preparation method as in step 1 and step 2 of example 2 except that the compounding ratio of the metals in step 1 was such that Al-22Cu-6Si-2Ni-Mg-0.1Ti-0.2Bi was used.
(II) the same preparation method as that of step 1 and step 2 of the example 2 is adopted, except that the proportion of the metal in the step 1 is Al-22Cu-6Si-Mg-0.1Ti-0.2Bi, and no nickel is added into the brazing filler metal, so that the aluminum alloy ingot is obtained.
And respectively sampling at the same position of the two cast ingots, and observing the microstructure of the cast ingots by adopting an Observer Al metallographic microscope. As a result, as shown in FIGS. 2 and 3, the white area in the metallographic micrograph was CuAl2An intermetallic compound. In the figure 3, Ni element is not added in the aluminum-based brazing filler metal, and a large amount of CuAl distributed in the cast ingot microstructure is obtained2The intermetallic compound is a hard and brittle phase, is in a fishbone shape, is difficult to break, has any direction, and is easy to crack in the rolling process of processing the foil strip. While figure shows2, Ni element is added into the aluminum-based brazing filler metal to ensure that CuAl in the cast ingot2The content of intermetallic compounds is reduced, and CuAl is generated due to the existence of Ni element2The intermetallic compound is in an oval block shape, and is easy to break during rolling, so that the foil strip is relatively easy to roll. Compared with the metallographic photographs of the ingot casting structures shown in the figures 2 and 3, the aluminum-based brazing filler metal is added with Ni element, so that CuAl in the brazing filler metal can be effectively changed2The form of the intermetallic compound reduces the brittleness of the brazing filler metal and improves the processing performance of the brazing filler metal.
In the above examples, which only exemplify the Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy foil-shaped brazing material of the present invention and the method for producing the same, the present invention is configured such that: the contents of copper, silicon, nickel and magnesium in the alloy components can be freely selected within the specified ranges, and are not listed here, so the technical scheme included in the above description should be regarded as illustrative and is not used to limit the protection scope of the present invention.
Claims (7)
1. A preparation method of Al-Cu-Si-Ni-Mg-Ti-Bi aluminum-based alloy solder is characterized by comprising the following steps of casting, centrifugal casting, superplastic treatment, isothermal rolling and cold rolling:
I. preparing materials: the purity of aluminum is more than 99.9 percent, the purity of copper is oxygen-free copper, the purity of silicon is more than 99.99 percent, the purity of nickel is more than 99.9 percent, the purity of magnesium is more than 99.99 percent, the purity of titanium is more than 99.99 percent, and the purity of bismuth is more than 99.99 percent; weighing the following raw materials in percentage by mass: 18-22 wt% of Cu, 5-7 wt% of Si, 1-5 wt% of Ni, 0.3-1 wt% of Mg, 0.1-0.2 wt% of Ti, 0.2-0.3 wt% of Bi and the balance of Al;
II, preparing an intermediate alloy:
(I) adding an aluminum ingot into a graphite crucible of a medium-frequency induction furnace, heating to melt the aluminum ingot, adding a copper ingot, heating the furnace to 750-800 ℃, fully stirring, casting a ingot after the copper ingot is completely melted, and casting the ingot at an alloy casting temperature of 700-750 ℃ to obtain an Al-Cu intermediate alloy;
(II) adding an aluminum ingot into a graphite crucible of the medium-frequency induction furnace, heating the graphite crucible to 800-850 ℃ after the aluminum ingot is melted, pressing polycrystalline silicon into aluminum liquid, keeping the temperature at 800-850 ℃ for 10-15 min after the polycrystalline silicon is completely melted down, fully stirring, casting ingots, and casting the alloys at the temperature of 850-900 ℃ to obtain Al-Si intermediate alloys;
(III) adding an aluminum ingot into a graphite crucible of a medium-frequency induction furnace, heating the graphite crucible to 1000-1050 ℃ after the aluminum ingot is melted, adding pure titanium, keeping the temperature at 1000-1050 ℃ for 10-15 min after the titanium is completely melted, fully stirring, casting ingots, and casting the alloys at 1050-1100 ℃ to obtain Al-Ti intermediate alloys;
and III, alloy casting: putting pure aluminum into a graphite crucible of a medium-frequency induction furnace, heating, sequentially adding Al-Cu, Al-Si, Al-Ti intermediate alloy and a pure nickel belt after aluminum ingots are completely melted, heating to 750-800 ℃ after the intermediate alloy and the nickel are completely melted, preserving heat for 10-15 min, pressing hexachloroethane into the bottom of alloy liquid by using a graphite cover, stirring, degassing, slagging, scattering a little refining agent which selects potassium fluoroaluminate, removing surface scum, heating to 650-700 ℃, adding magnesium and bismuth, fully stirring, and casting to obtain cast ingots;
IV, centrifugal casting: crushing the cast brazing filler metal ingot, putting the crushed cast brazing filler metal ingot into a graphite crucible in a centrifugal casting furnace, melting the crushed cast brazing filler metal ingot under the protection of Ar gas, heating the ingot to 650-700 ℃ after the ingot is completely melted, and casting the ingot into a sheet with the thickness of 1.5-2.5 mm by adopting a centrifugal casting mode;
v, superplasticizing treatment: placing the sheet obtained in the step IV into a resistance furnace, preserving heat for 12-16 hours at 400-420 ℃, then heating to 480-490 ℃, preserving heat for 30-45 min, and quenching;
VI, isothermal rolling: c, heating the plate blank obtained in the step V at the temperature of 450-460 ℃, rolling the plate blank at the temperature of 450-460 ℃ by a rolling mill, and carrying out isothermal rolling with the pass processing rate of 3-5% to obtain a strip with the thickness of 0.5-0.7 mm;
VII, cold rolling: cold rolling the strip subjected to isothermal rolling at the temperature of 5-50 ℃, and then annealing at the temperature of 420-450 ℃ for 1.5-2 h; and (4) cold rolling in multiple times until the required thickness is obtained.
2. The preparation method according to claim 1, wherein the brazing filler metal obtained in the step VII is a foil-shaped brazing filler metal, and the thickness of the brazing filler metal is 0.03-0.15 mm.
3. The method of claim 1, wherein the Al-Cu master alloy in the step II has a copper content of 50 wt%, the Al-Si master alloy has a silicon content of 30 wt%, and the Al-Ti master alloy has a titanium content of 5 wt%.
4. The method of claim 1, wherein the hexachloroethane is used in an amount of 0.3 to 0.4 wt% and the refining agent is used in an amount of 0.2 to 0.3 wt% based on the amount of the furnace in step III.
5. The manufacturing method according to claim 1, wherein the cold rolling pass reduction rate in the step VII is controlled to be 3-5%, and the total cold rolling reduction rate is 9-15%.
6. An Al-Cu-Si-Ni-Mg-Ti-Bi aluminum based alloyed solder, characterized in that it is produced by the method according to any one of claims 1 to 5.
7. Use of an Al-Cu-Si-Ni-Mg-Ti-Bi aluminium based alloy solder according to claim 6 in low temperature or staged vacuum brazing of 3A21, 2A50, 6063 and 6061 aluminium alloys and in vacuum brazing of aluminium-copper dissimilar metals.
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| JP3168227B2 (en) * | 1992-06-26 | 2001-05-21 | 日本発条株式会社 | Brazing filler metal for aluminum alloy and brazed joint |
| CN1088496A (en) * | 1992-12-19 | 1994-06-29 | 中国石油化工总公司发展部 | Electromagnetic certrifugal casting technology |
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