CN103846570A - Preparation method of silver-based brazing filler metal for brazing high-volume-fraction SiC particle reinforced aluminum matrix composites - Google Patents
Preparation method of silver-based brazing filler metal for brazing high-volume-fraction SiC particle reinforced aluminum matrix composites Download PDFInfo
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- CN103846570A CN103846570A CN201410081894.1A CN201410081894A CN103846570A CN 103846570 A CN103846570 A CN 103846570A CN 201410081894 A CN201410081894 A CN 201410081894A CN 103846570 A CN103846570 A CN 103846570A
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- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 239000002245 particle Substances 0.000 title claims abstract description 30
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000005219 brazing Methods 0.000 title abstract description 19
- 229910052751 metal Inorganic materials 0.000 title abstract description 12
- 239000002184 metal Substances 0.000 title abstract description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title abstract description 8
- 239000004332 silver Substances 0.000 title abstract description 8
- 239000011159 matrix material Substances 0.000 title abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 title abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title abstract description 5
- 239000000945 filler Substances 0.000 title abstract 7
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 80
- 239000000956 alloy Substances 0.000 claims abstract description 80
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229910008839 Sn—Ti Inorganic materials 0.000 claims abstract description 38
- 239000010453 quartz Substances 0.000 claims abstract description 35
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052786 argon Inorganic materials 0.000 claims abstract description 28
- 229910052802 copper Inorganic materials 0.000 claims abstract description 27
- 239000010949 copper Substances 0.000 claims abstract description 27
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 230000006698 induction Effects 0.000 claims abstract description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910000679 solder Inorganic materials 0.000 claims description 74
- 229910017944 Ag—Cu Inorganic materials 0.000 claims description 32
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 31
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 30
- 238000003723 Smelting Methods 0.000 claims description 26
- 239000003708 ampul Substances 0.000 claims description 26
- 239000007789 gas Substances 0.000 claims description 26
- 238000002844 melting Methods 0.000 claims description 25
- 230000008018 melting Effects 0.000 claims description 25
- 238000005476 soldering Methods 0.000 claims description 23
- 229910052738 indium Inorganic materials 0.000 claims description 19
- 229910052718 tin Inorganic materials 0.000 claims description 19
- 229910052719 titanium Inorganic materials 0.000 claims description 19
- 238000005275 alloying Methods 0.000 claims description 16
- 239000008188 pellet Substances 0.000 claims description 16
- 238000012360 testing method Methods 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 15
- 239000012634 fragment Substances 0.000 claims description 12
- 229910017945 Cu—Ti Inorganic materials 0.000 claims description 8
- 229910001128 Sn alloy Inorganic materials 0.000 claims description 8
- 238000005336 cracking Methods 0.000 claims description 8
- 238000010891 electric arc Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 230000005611 electricity Effects 0.000 claims description 4
- 229910001651 emery Inorganic materials 0.000 claims description 4
- 238000010297 mechanical methods and process Methods 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 11
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 238000004100 electronic packaging Methods 0.000 abstract description 2
- 150000002739 metals Chemical class 0.000 abstract 1
- 229910000833 kovar Inorganic materials 0.000 description 11
- 239000000463 material Substances 0.000 description 11
- 238000003466 welding Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 230000002708 enhancing effect Effects 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229910000553 6063 aluminium alloy Inorganic materials 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- 238000007499 fusion processing Methods 0.000 description 2
- 210000004209 hair Anatomy 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000010183 spectrum analysis Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- UJXVAJQDLVNWPS-UHFFFAOYSA-N [Al].[Al].[Al].[Fe] Chemical compound [Al].[Al].[Al].[Fe] UJXVAJQDLVNWPS-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000010406 interfacial reaction Methods 0.000 description 1
- 229910021326 iron aluminide Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
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- 239000002893 slag Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag 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
- B23K35/40—Making wire or rods for soldering or welding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
Abstract
The invention relates to a preparation method of a silver-based brazing filler metal for brazing high-volume-fraction SiC particle reinforced aluminum matrix composites. The purpose of the invention is to solve the problems that brazing filler metals within the temperature range between 565 DEG C and 585 DEG C do not exist in the field of electronic packaging at present and that the strength of weld joints is low. The method includes the following steps: (1) Ag-Cu-In-Sn-Ti alloy balls which are uniformly mixed are prepared; (2) oxide layers are removed, and the balls are broken into alloy blocks; (3) the alloy blocks are put into a quartz tube with a bottom slot, so that a quartz tube loaded with the alloy blocks is obtained; (4) the quartz tube loaded with the alloy blocks is put into the heating induction coil of a melt-spun furnace, and high-purity argon is filled after vacuumization; (5) when the Ag-Cu-In-Sn-Ti alloy blocks in the quartz tube are heated to melt, argon is utilized to blow the melted brazing filler metal out of the bottom slot of the quartz tube, the melted brazing filler metal sputters onto a copper roller, so that a strip is thrown out, and after cooling, the silver-based brazing filler metal is obtained. The preparation method is mainly used for preparing the silver-based brazing filler metal.
Description
Technical field
The present invention relates to a kind of preparation method of solder of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material.
Background technology
Enhancing aluminum-base composite material by silicon carbide particles has the excellent properties such as high specific strength, specific stiffness, dimensional stability, designability and wear-resisting, corrosion-resistant, resistance to ray because of it, particularly raw material sources fully, low cost of manufacture, market be acceptant, be the widest new structural material of application potential in metal-base composites, can be widely used in the industrial fields such as Aero-Space, automobile making, instrument and meter, electronic information, precision optical machinery.But the applying of this new structural material but run into that a Pinch technology difficult problem---weldability is very poor.This is the greatest differences due to wild phase and alloy matrix aluminum physical and chemical performance, it is extremely difficult obtaining high-quality welding point by melting method, very easily produce pore, slag inclusion, the defect such as loose, lack of penetration, simultaneously under welding high-temperature condition, carborundum will with aluminium liquid generation interfacial reaction, generate C
3al
4needle-like hazardous compound, strength of joint is very low.In recent years, the human hairs such as ox Jinan-Tai'an understand the diffusion welding (DW), vacuum brazing, furnace brazing, resistance-welding process of enhancing aluminum-base composite material by silicon carbide particles etc. and have obtained multinomial national inventing patent, open up new Research Thinking, although having realized composite under vacuum condition is connected with the effective of kovar alloy, but between solder and kovar alloy, generate more iron aluminide fragility phase, weakened strength of joint.The human hairs such as the Yan Jiuchun of Harbin Institute of Technology understand about the technique such as vibration weldering, ultrasonic wave fine welding of aluminum matrix composite and are successfully applied to space structure connection, but for the very harsh high-end product of Service Environment, welding quality still needs further to be improved.Its basic reason be composite material surface exposed a large amount of SiC ceramic enhancement phase, it contains ionic bond and covalent bond, be difficult to be soaked by the solder of containing metal key, brought great difficulty to brazing process, further develop more efficiently brazing solder imperative.
Summary of the invention
The present invention will solve current Electronic Packaging field without 565 ℃～585 ℃ temperature range solders and the low problem of weld strength, and a kind of preparation method of silver-base solder of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material is provided.
A kind of preparation method of silver-base solder of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material completes according to the following steps:
One, take raw material by mass percent 45～50%Ag, 16～20%Cu, 16～20%In, 15～18%Sn and 0.5～1.5%Ti;
Two, 45～50%Ag step 1 being taken and 16～20%Cu are placed in high-frequency induction vacuum melting furnace, be 1Pa in vacuum, smelting temperature is melting 15min～20min under the condition of 1350 ℃, after air cooling, obtain Ag-Cu intermediate alloy, by Ag-Cu intermediate alloy in two, obtain Ag-Cu intermediate alloy A and Ag-Cu intermediate alloy B, and the mass ratio of described Ag-Cu intermediate alloy A and Ag-Cu intermediate alloy B is 1:1;
Three, the Ag-Cu intermediate alloy A, 16～20%In and the 15～18%Sn that step 1 takes that in high-frequency induction vacuum melting furnace, add step 2 to obtain, be 1Pa in vacuum, smelting temperature is melting 5min～10min under the condition of 850 ℃, obtains Ag-Cu-In-Sn alloy after air cooling;
Four, then the Ag-Cu intermediate alloy B and the 0.5～1.5%Ti that in vacuum non-consumable electric arc smelting furnace, add step 2 to obtain are 4 × 10 by being evacuated to absolute pressure in vacuum chamber
-3pa, then to be filled with high-purity argon gas to vacuum chamber relative pressure be-0.04MPa～-0.02MPa, is melting 5min～10min under the condition of 1750 ℃ at smelting temperature, obtains Ag-Cu-Ti intermediate alloy after air cooling;
Five, then the Ag-Cu-Ti intermediate alloy that adds Ag-Cu-In-Sn alloy that step 3 obtains and step 4 to obtain in vacuum non-consumable electric arc smelting furnace is 4 × 10 by being evacuated to absolute pressure in vacuum chamber
-3pa, then to be filled with high-purity argon gas to vacuum chamber relative pressure be-0.04MPa～-0.02MPa, is melting 5min～10min under the condition of 1750 ℃ at smelting temperature, obtains the Ag-Cu-In-Sn-Ti alloying pellet mixing after air cooling;
Six, adopt emery wheel to polish to the Ag-Cu-In-Sn-Ti alloying pellet mixing, remove the oxide layer on Ag-Cu-In-Sn-Ti alloying pellet surface, then by Mechanical Method, the Ag-Cu-In-Sn-Ti alloying pellet after polishing is broken into the Ag-Cu-In-Sn-Ti alloy block that size is less than 30mm;
Cracking in the bottom of the quartz test tube that is seven, 30mm to internal diameter, stitches wide 0.4mm, and the Ag-Cu-In-Sn-Ti alloy block that then size is less than to 30mm is put into the quartz ampoule cracking in bottom, obtains being equipped with the quartz ampoule of Ag-Cu-In-Sn-Ti alloy fragment;
Eight, the quartz ampoule that Ag-Cu-In-Sn-Ti alloy fragment is housed is put into the heat induced coil getting rid of with machine, then getting rid of band machine inner chamber, to be evacuated to absolute pressure be 4 × 10
-3pa, then be filled with high-purity argon gas to getting rid of band machine inner chamber relative pressure for-0.07MPa～-0.04MPa;
Nine, get rid of the heat induced coil electricity with machine, in the time that the Ag-Cu-In-Sn-Ti alloy fragment in quartz ampoule is heated to molten condition, open the air accumulator getting rid of with machine, under take relative pressure as-0.05MPa～-0.02MPa, pass into argon gas to quartz ampoule, utilize argon gas that the solder of molten condition is blown out from gap, quartz ampoule bottom, being splashed to rotating speed is on the copper roller of 20m/s～40m/s, and throwing away thickness is the strip of 30 μ m～80 μ m, can obtain silver-base solder after cooling.
Advantage of the present invention: one, the invention provides a kind of high-volume fractional silicon-carbide particle reinforced aluminium-base composite material self connection and the Novel silver-based solder with kovar alloy dissimilar material solder brazing thereof, further to improve joint quality, this kind of solder also expanded the scope of application of solder to mother metal kind simultaneously, and simplifies soldering processes; The silver-base solder of preparation is Ag47-Cu18-In17-Sn17-Ti1 solder, and its solidus is that 475 ℃, liquidus curve are 530 ℃.The matrix of welded composite can be not only A356 aluminium alloy but also can be 6063 aluminium alloys that contain more magnesium and a certain amount of silicon; Not only be applicable to the connection between high-volume fractional silicon-carbide particle reinforced aluminium-base composite material self, be also applicable to being connected between high-volume fractional silicon-carbide particle reinforced aluminium-base composite material and kovar alloy; And compared with patent Zl200910073339-3, silver-base solder not with kovar alloy generation chemical reaction production fragility phase, heating temperature wide ranges is 565 ℃～585 ℃, more than being used in mother metal solidus; Compared with patent Zl200910073340-6, do not need weldering front in composite material surface nickel plating, need to be at solder coating on both sides brazing flux when welding yet, the resistance to corrosion of zinc-based solder weld seam is not as silver-base solder in addition.
Two, adopt vacuum to get rid of band legal system and make silver-based material, though for routine techniques means never people utilize vacuum to get rid of the solder of making soldering enhancing aluminum-base composite material by silicon carbide particles with legal system, and good silver-base solder has great difficulty to get rid of into plasticity, the one, material composition, the 2nd, the requirement of solder fusion process is strict, the 3rd, belt-rejecting technology parameter complexity, influence factor is a lot, the present invention is from the theoretical Scientific Establishment solder composition that combines with experiment, the strict solder smelting process of controlling, optimize foil-shaped brazing material and get rid of band parameter, successfully prepare the silver-base solder that soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material self connects and is connected with kovar alloy.
Accompanying drawing explanation
Fig. 1 is the silver-base solder photo in kind that test one makes;
Fig. 2 is the microscopic appearance figure of test one silver-base solder making;
Fig. 3 is the energy spectrum analysis figure of test one silver-base solder making;
Fig. 4 is the dsc analysis curve map of test one silver-base solder making.
The specific embodiment
The specific embodiment one: present embodiment is that a kind of preparation method of silver-base solder of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material completes according to the following steps:
One, take raw material by mass percent 45～50%Ag, 16～20%Cu, 16～20%In, 15～18%Sn and 0.5～1.5%Ti; The purity of described Ag, Cu, In, Sn and Ti is greater than 99%;
Two, 45～50%Ag step 1 being taken and 16～20%Cu are placed in high-frequency induction vacuum melting furnace, be 1Pa in vacuum, smelting temperature is melting 15min～20min under the condition of 1350 ℃, after air cooling, obtain Ag-Cu intermediate alloy, by Ag-Cu intermediate alloy in two, obtain Ag-Cu intermediate alloy A and Ag-Cu intermediate alloy B, and the mass ratio of described Ag-Cu intermediate alloy A and Ag-Cu intermediate alloy B is 1:1;
Three, the Ag-Cu intermediate alloy A, 16～20%In and the 15～18%Sn that step 1 takes that in high-frequency induction vacuum melting furnace, add step 2 to obtain, be 1Pa in vacuum, smelting temperature is melting 5min～10min under the condition of 850 ℃, obtains Ag-Cu-In-Sn alloy after air cooling;
Four, then the Ag-Cu intermediate alloy B and the 0.5～1.5%Ti that in vacuum non-consumable electric arc smelting furnace, add step 2 to obtain are 4 × 10 by being evacuated to absolute pressure in vacuum chamber
-3pa, then to be filled with high-purity argon gas to vacuum chamber relative pressure be-0.04MPa～-0.02MPa, is melting 5min～10min under the condition of 1750 ℃ at smelting temperature, obtains Ag-Cu-Ti intermediate alloy after air cooling;
Five, then the Ag-Cu-Ti intermediate alloy that adds Ag-Cu-In-Sn alloy that step 3 obtains and step 4 to obtain in vacuum non-consumable electric arc smelting furnace is 4 × 10 by being evacuated to absolute pressure in vacuum chamber
-3pa, then to be filled with high-purity argon gas to vacuum chamber relative pressure be-0.04MPa～-0.02MPa, is melting 5min～10min under the condition of 1750 ℃ at smelting temperature, obtains the Ag-Cu-In-Sn-Ti alloying pellet mixing after air cooling;
Six, adopt emery wheel to polish to the Ag-Cu-In-Sn-Ti alloying pellet mixing, remove the oxide layer on Ag-Cu-In-Sn-Ti alloying pellet surface, then by Mechanical Method, the Ag-Cu-In-Sn-Ti alloying pellet after polishing is broken into the Ag-Cu-In-Sn-Ti alloy block that size is less than 30mm;
Cracking in the bottom of the quartz test tube that is seven, 30mm to internal diameter, stitches wide 0.4mm, and the Ag-Cu-In-Sn-Ti alloy block that then size is less than to 30mm is put into the quartz ampoule cracking in bottom, obtains being equipped with the quartz ampoule of Ag-Cu-In-Sn-Ti alloy fragment;
Eight, the quartz ampoule that Ag-Cu-In-Sn-Ti alloy fragment is housed is put into the heat induced coil getting rid of with machine, then getting rid of band machine inner chamber, to be evacuated to absolute pressure be 4 × 10
-3pa, then be filled with high-purity argon gas to getting rid of band machine inner chamber relative pressure for-0.07MPa～-0.04MPa;
Nine, get rid of the heat induced coil electricity with machine, in the time that the Ag-Cu-In-Sn-Ti alloy fragment in quartz ampoule is heated to molten condition, open the air accumulator getting rid of with machine, under take relative pressure as-0.05MPa～-0.02MPa, pass into argon gas to quartz ampoule, utilize argon gas that the solder of molten condition is blown out from gap, quartz ampoule bottom, being splashed to rotating speed is on the copper roller of 20m/s～40m/s, and throwing away thickness is the strip of 30 μ m～80 μ m, can obtain silver-base solder after cooling.
Present embodiment provides a kind of high-volume fractional silicon-carbide particle reinforced aluminium-base composite material self connection and the Novel silver-based solder with kovar alloy dissimilar material solder brazing thereof, further to improve joint quality, this kind of solder also expanded the scope of application of solder to mother metal kind simultaneously, and simplifies soldering processes; The silver-base solder of preparation is Ag47-Cu18-In17-Sn17-Ti1 solder, and its solidus is that 475 ℃, liquidus curve are 530 ℃.The matrix of welded composite can be not only A356 aluminium alloy but also can be 6063 aluminium alloys that contain more magnesium and a certain amount of silicon; Not only be applicable to the connection between high-volume fractional silicon-carbide particle reinforced aluminium-base composite material self, be also applicable to being connected between high-volume fractional silicon-carbide particle reinforced aluminium-base composite material and kovar alloy; And compared with patent Zl200910073339-3, silver-base solder not with kovar alloy generation chemical reaction production fragility phase, heating temperature wide ranges is 565 ℃～585 ℃, more than being used in mother metal solidus; Compared with patent Zl200910073340-6, do not need weldering front in composite material surface nickel plating, need to be at solder coating on both sides brazing flux when welding yet, the resistance to corrosion of zinc-based solder weld seam is not as silver-base solder in addition.
In present embodiment, adopt vacuum to get rid of band legal system and make silver-based material, though for routine techniques means never people utilize vacuum to get rid of the solder of making soldering enhancing aluminum-base composite material by silicon carbide particles with legal system, and good silver-base solder has great difficulty to get rid of into plasticity, the one, material composition, the 2nd, the requirement of solder fusion process is strict, the 3rd, belt-rejecting technology parameter complexity, influence factor is a lot, present embodiment is from the theoretical Scientific Establishment solder composition that combines with experiment, the strict solder smelting process of controlling, optimize foil-shaped brazing material and get rid of band parameter, successfully prepare the silver-base solder that soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material self connects and is connected with kovar alloy.
The specific embodiment two: present embodiment is different from the specific embodiment one: step 1 takes raw material by mass percent 46%Ag, 19%Cu, 18%In, 16%Sn and 1%Ti.Other are identical with the specific embodiment one.
The specific embodiment three: present embodiment is different from the specific embodiment one or two: step 1 takes raw material by mass percent 48%Ag, 17%Cu, 16%In, 18%Sn and 1%Ti.Other are identical with the specific embodiment one or two.
The specific embodiment four: present embodiment is different from the specific embodiment one to three: step 1 takes raw material by mass percent 47%Ag, 18%Cu, 17%In, 17%Sn and 1%Ti.Other are identical with the specific embodiment one to three.
The specific embodiment five: present embodiment is different from one of specific embodiment one to four: step 1 takes raw material by mass percent 47.5%Ag, 17.5%Cu, 18%In, 16%Sn and 1%Ti.Other are identical with one of specific embodiment one to four.
The specific embodiment six: present embodiment is different from one of specific embodiment one to five: step 1 takes raw material by mass percent 50%Ag, 16%Cu, 16%In, 17%Sn and 1%Ti.Other are identical with one of specific embodiment one to five.
The specific embodiment seven: present embodiment is different from one of specific embodiment one to six: step 5 is filled with high-purity argon gas to vacuum chamber relative pressure and is-0.03MPa.Other are identical with one of specific embodiment one to six.
The specific embodiment eight: present embodiment is different from one of specific embodiment one to seven: step 8 is filled with high-purity argon gas and to getting rid of band machine inner chamber relative pressure is-0.05MPa.Other are identical with one of specific embodiment one to seven.
The specific embodiment nine: present embodiment is different from one of specific embodiment one to eight: step 9 passes into argon gas to quartz ampoule under take relative pressure as-0.03MPa.Other are identical with one of specific embodiment one to eight.
The specific embodiment ten: present embodiment is different from one of specific embodiment one to nine: step 9 is splashed on the copper roller that rotating speed is 30m/s, throws away the strip that thickness is 50 μ m.Other are identical with one of specific embodiment one to nine.
Adopt following verification experimental verification effect of the present invention:
Test one: one, take raw material by mass percent 47%Ag, 18%Cu, 17%In, 17%Sn and 1%Ti;
Two, 47%Ag step 1 being taken and 18%Cu are placed in high-frequency induction vacuum melting furnace, be 1Pa in vacuum, smelting temperature is melting 20min under the condition of 1350 ℃, after air cooling, obtain Ag-Cu intermediate alloy, by Ag-Cu intermediate alloy in two, obtain Ag-Cu intermediate alloy A and Ag-Cu intermediate alloy B, and the mass ratio of described Ag-Cu intermediate alloy A and Ag-Cu intermediate alloy B is 1:1;
Three, the Ag-Cu intermediate alloy A, 17%In and the 17%Sn that step 1 takes that in high-frequency induction vacuum melting furnace, add step 2 to obtain, be 1Pa in vacuum, and smelting temperature is melting 10min under the condition of 850 ℃, obtains Ag-Cu-In-Sn alloy after air cooling;
Four, then the Ag-Cu intermediate alloy B and the 1%Ti that in vacuum non-consumable electric arc smelting furnace, add step 2 to obtain are 4 × 10 by being evacuated to absolute pressure in vacuum chamber
-3pa, then to be filled with high-purity argon gas to vacuum chamber relative pressure be-0.03MPa, is melting 10min under the condition of 1750 ℃ at smelting temperature, obtains Ag-Cu-Ti intermediate alloy after air cooling;
Five, then the Ag-Cu-Ti intermediate alloy that adds Ag-Cu-In-Sn alloy that step 3 obtains and step 4 to obtain in vacuum non-consumable electric arc smelting furnace is 4 × 10 by being evacuated to absolute pressure in vacuum chamber
-3pa, then to be filled with high-purity argon gas to vacuum chamber relative pressure be-0.03MPa, is melting 10min under the condition of 1750 ℃ at smelting temperature, obtains the Ag-Cu-In-Sn-Ti alloying pellet mixing after air cooling;
Six, adopt emery wheel to polish to the Ag-Cu-In-Sn-Ti alloying pellet mixing, remove the oxide layer on Ag-Cu-In-Sn-Ti alloying pellet surface, then by Mechanical Method, the Ag-Cu-In-Sn-Ti alloying pellet after polishing is broken into the Ag-Cu-In-Sn-Ti alloy block that size is less than 30mm;
Cracking in the bottom of the quartz test tube that is seven, 30mm to internal diameter, stitches wide 0.4mm, and the Ag-Cu-In-Sn-Ti alloy block that then size is less than to 30mm is put into the quartz ampoule cracking in bottom, obtains being equipped with the quartz ampoule of Ag-Cu-In-Sn-Ti alloy fragment;
Eight, the quartz ampoule that Ag-Cu-In-Sn-Ti alloy fragment is housed is put into the heat induced coil getting rid of with machine, then getting rid of band machine inner chamber, to be evacuated to absolute pressure be 4 × 10
-3pa, then be filled with high-purity argon gas to getting rid of band machine inner chamber relative pressure for-0.05MPa;
Nine, get rid of the heat induced coil electricity with machine, in the time that the Ag-Cu-In-Sn-Ti alloy fragment in quartz ampoule is heated to molten condition, open the air accumulator getting rid of with machine, under take relative pressure as-0.03MPa, pass into argon gas to quartz ampoule, utilize argon gas that the solder of molten condition is blown out from gap, quartz ampoule bottom, being splashed to rotating speed is on the copper roller of 30m/s, throws away the strip that thickness is 50 μ m, can obtain silver-base solder after cooling.
Be to be incubated 30min, soldering high volume fraction grain enhanced aluminum-base compound material (55%SiC under 585 ℃, the vacuum condition that is 10-3Pa by test one silver-base solder making in temperature
p/ 6063) with kovar alloy electronic package shell, shear strength can reach 97MPa, and leak rate is 10
-10pa.m
3/ s, meets sealing requirements.
Fig. 1 is the silver-base solder photo in kind that test one makes, and is within the scope of 20m/s～40m/s as can be seen from Figure 1 in copper roller surface rotational line speed, and the solder appearance forming obtaining under different rotating speeds is all good;
Fig. 2 is the microscopic appearance figure of test one silver-base solder making, and smooth surface, even, fine and close as can be seen from Figure 2 continuously, does not have the shortcoming such as bubble, assorted point.
Fig. 3 is the energy spectrum analysis figure of test one silver-base solder making, and table 1, for the test one silver-base solder element wt percentage making and atomicity percentage, can find out that from Fig. 3 and table 1 the silver-base solder percentage composition making is consistent with design data.
Table 1: the test one silver-base solder element wt percentage making and atomicity percentage
| Element | Mass percent | Atomic percent |
| AgL | 46.90 | 42.22 |
| InL | 18.28 | 15.46 |
| SnL | 15.84 | 12.96 |
| TiK | 00.67 | 01.35 |
| CuK | 18.32 | 28.01 |
Fig. 4 is the dsc analysis curve map of test one silver-base solder making, and the silver-base solder solid-liquid phase line making is as can be seen from Figure 4 respectively 475 ℃ and 530 ℃.
Claims (10)
1. a preparation method for the silver-base solder of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material, is characterized in that the preparation method of the silver-base solder of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material completes according to the following steps:
One, take raw material by mass percent 45～50%Ag, 16～20%Cu, 16～20%In, 15～18%Sn and 0.5～1.5%Ti;
Two, 45～50%Ag step 1 being taken and 16～20%Cu are placed in high-frequency induction vacuum melting furnace, be 1Pa in vacuum, smelting temperature is melting 15min～20min under the condition of 1350 ℃, after air cooling, obtain Ag-Cu intermediate alloy, by Ag-Cu intermediate alloy in two, obtain Ag-Cu intermediate alloy A and Ag-Cu intermediate alloy B, and the mass ratio of described Ag-Cu intermediate alloy A and Ag-Cu intermediate alloy B is 1:1;
Three, the Ag-Cu intermediate alloy A, 16～20%In and the 15～18%Sn that step 1 takes that in high-frequency induction vacuum melting furnace, add step 2 to obtain, be 1Pa in vacuum, smelting temperature is melting 5min～10min under the condition of 850 ℃, obtains Ag-Cu-In-Sn alloy after air cooling;
Four, then the Ag-Cu intermediate alloy B and the 0.5～1.5%Ti that in vacuum non-consumable electric arc smelting furnace, add step 2 to obtain are 4 × 10 by being evacuated to absolute pressure in vacuum chamber
-3pa, then to be filled with high-purity argon gas to vacuum chamber relative pressure be-0.04MPa～-0.02MPa, is melting 5min～10min under the condition of 1750 ℃ at smelting temperature, obtains Ag-Cu-Ti intermediate alloy after air cooling;
Five, then the Ag-Cu-Ti intermediate alloy that adds Ag-Cu-In-Sn alloy that step 3 obtains and step 4 to obtain in vacuum non-consumable electric arc smelting furnace is 4 × 10 by being evacuated to absolute pressure in vacuum chamber
-3pa, then to be filled with high-purity argon gas to vacuum chamber relative pressure be-0.04MPa～-0.02MPa, is melting 5min～10min under the condition of 1750 ℃ at smelting temperature, obtains the Ag-Cu-In-Sn-Ti alloying pellet mixing after air cooling;
Six, adopt emery wheel to polish to the Ag-Cu-In-Sn-Ti alloying pellet mixing, remove the oxide layer on Ag-Cu-In-Sn-Ti alloying pellet surface, then by Mechanical Method, the Ag-Cu-In-Sn-Ti alloying pellet after polishing is broken into the Ag-Cu-In-Sn-Ti alloy block that size is less than 30mm;
Cracking in the bottom of the quartz test tube that is seven, 30mm to internal diameter, stitches wide 0.4mm, and the Ag-Cu-In-Sn-Ti alloy block that then size is less than to 30mm is put into the quartz ampoule cracking in bottom, obtains being equipped with the quartz ampoule of Ag-Cu-In-Sn-Ti alloy fragment;
Eight, the quartz ampoule that Ag-Cu-In-Sn-Ti alloy fragment is housed is put into the heat induced coil getting rid of with machine, then getting rid of band machine inner chamber, to be evacuated to absolute pressure be 4 × 10
-3pa, then be filled with high-purity argon gas to getting rid of band machine inner chamber relative pressure for-0.07MPa～-0.04MPa;
Nine, get rid of the heat induced coil electricity with machine, in the time that the Ag-Cu-In-Sn-Ti alloy fragment in quartz ampoule is heated to molten condition, open the air accumulator getting rid of with machine, under take relative pressure as-0.05MPa～-0.02MPa, pass into argon gas to quartz ampoule, utilize argon gas that the solder of molten condition is blown out from gap, quartz ampoule bottom, being splashed to rotating speed is on the copper roller of 20m/s～40m/s, and throwing away thickness is the strip of 30 μ m～80 μ m, can obtain silver-base solder after cooling.
2. the preparation method of the silver-base solder of a kind of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material according to claim 1, is characterized in that step 1 takes raw material by mass percent 46%Ag, 19%Cu, 18%In, 16%Sn and 1%Ti.
3. the preparation method of the silver-base solder of a kind of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material according to claim 1, is characterized in that step 1 takes raw material by mass percent 48%Ag, 17%Cu, 16%In, 18%Sn and 1%Ti.
4. the preparation method of the silver-base solder of a kind of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material according to claim 1, is characterized in that step 1 takes raw material by mass percent 47%Ag, 18%Cu, 17%In, 17%Sn and 1%Ti.
5. the preparation method of the silver-base solder of a kind of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material according to claim 1, is characterized in that step 1 takes raw material by mass percent 47.5%Ag, 17.5%Cu, 18%In, 16%Sn and 1%Ti.
6. the preparation method of the silver-base solder of a kind of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material according to claim 1, is characterized in that step 1 takes raw material by mass percent 50%Ag, 16%Cu, 16%In, 17%Sn and 1%Ti.
7. the preparation method of the silver-base solder of a kind of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material according to claim 1, is characterized in that step 5 is filled with high-purity argon gas to vacuum chamber relative pressure and is-0.03MPa.
8. the preparation method of the silver-base solder of a kind of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material according to claim 1, is characterized in that step 8 is filled with high-purity argon gas and to getting rid of band machine inner chamber relative pressure is-0.05MPa.
9. the preparation method of the silver-base solder of a kind of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material according to claim 1, is characterized in that passing into argon gas to quartz ampoule under step 9 is take relative pressure as-0.03MPa.
10. the preparation method of the silver-base solder of a kind of soldering high-volume fractional silicon-carbide particle reinforced aluminium-base composite material according to claim 1, is characterized in that step 9 is splashed on the copper roller that rotating speed is 30m/s, throws away the strip that thickness is 50 μ m.
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| CN110691762A (en) * | 2017-05-30 | 2020-01-14 | 电化株式会社 | Ceramic circuit board and method for manufacturing the same |
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| CN108480876A (en) * | 2018-03-30 | 2018-09-04 | 西安瑞鑫科金属材料有限责任公司 | A kind of silver-base solder for zirconia ceramics and solder bonding metal |
| CN110125510A (en) * | 2019-05-16 | 2019-08-16 | 哈尔滨瀚霖科技开发有限公司 | It is used to prepare the resistance brazing connection method of long size hard alloy |
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