CN114055012A - Multi-element copper-based alloy brazing filler metal containing rare earth elements, preparation method and brazing method thereof - Google Patents
Multi-element copper-based alloy brazing filler metal containing rare earth elements, preparation method and brazing method thereof Download PDFInfo
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- CN114055012A CN114055012A CN202111414453.5A CN202111414453A CN114055012A CN 114055012 A CN114055012 A CN 114055012A CN 202111414453 A CN202111414453 A CN 202111414453A CN 114055012 A CN114055012 A CN 114055012A
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- 238000005219 brazing Methods 0.000 title claims abstract description 118
- 239000010949 copper Substances 0.000 title claims abstract description 90
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 86
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 85
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 76
- 239000002184 metal Substances 0.000 title claims abstract description 76
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 75
- 239000000956 alloy Substances 0.000 title claims abstract description 75
- 239000000945 filler Substances 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 229910000679 solder Inorganic materials 0.000 claims abstract description 84
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 32
- 239000011135 tin Substances 0.000 claims abstract description 32
- 239000010936 titanium Substances 0.000 claims abstract description 32
- 229910052718 tin Inorganic materials 0.000 claims abstract description 27
- 229910052733 gallium Inorganic materials 0.000 claims abstract description 26
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 26
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims abstract description 25
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 25
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 36
- 229910000831 Steel Inorganic materials 0.000 claims description 36
- 239000010959 steel Substances 0.000 claims description 36
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 238000003723 Smelting Methods 0.000 claims description 18
- 238000010438 heat treatment Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- 230000006698 induction Effects 0.000 claims description 14
- 238000004140 cleaning Methods 0.000 claims description 13
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- 229910001069 Ti alloy Inorganic materials 0.000 claims description 12
- 238000005266 casting Methods 0.000 claims description 12
- IUYOGGFTLHZHEG-UHFFFAOYSA-N copper titanium Chemical compound [Ti].[Cu] IUYOGGFTLHZHEG-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 239000000758 substrate Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 7
- 239000011159 matrix material Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 5
- 238000003892 spreading Methods 0.000 claims description 4
- 230000007480 spreading Effects 0.000 claims description 4
- 239000003082 abrasive agent Substances 0.000 claims description 2
- 229910003460 diamond Inorganic materials 0.000 abstract description 59
- 239000010432 diamond Substances 0.000 abstract description 59
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 230000003685 thermal hair damage Effects 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 30
- 230000008018 melting Effects 0.000 description 24
- 238000002844 melting Methods 0.000 description 24
- 239000002994 raw material Substances 0.000 description 14
- 238000010586 diagram Methods 0.000 description 12
- 238000010891 electric arc Methods 0.000 description 12
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 12
- 229910052779 Neodymium Inorganic materials 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- 230000005496 eutectics Effects 0.000 description 7
- 229910018487 Ni—Cr Inorganic materials 0.000 description 6
- 229910000858 La alloy Inorganic materials 0.000 description 5
- FQVNUZAZHHOJOH-UHFFFAOYSA-N copper lanthanum Chemical compound [Cu].[La] FQVNUZAZHHOJOH-UHFFFAOYSA-N 0.000 description 5
- 229910052746 lanthanum Inorganic materials 0.000 description 5
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 4
- 239000012856 weighed raw material Substances 0.000 description 4
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 229910017945 Cu—Ti Inorganic materials 0.000 description 3
- AHGIVYNZKJCSBA-UHFFFAOYSA-N [Ti].[Ag].[Cu] Chemical compound [Ti].[Ag].[Cu] AHGIVYNZKJCSBA-UHFFFAOYSA-N 0.000 description 3
- KCGHDPMYVVPKGJ-UHFFFAOYSA-N [Ti].[Cu].[Sn] Chemical compound [Ti].[Cu].[Sn] KCGHDPMYVVPKGJ-UHFFFAOYSA-N 0.000 description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- VNNRSPGTAMTISX-UHFFFAOYSA-N chromium nickel Chemical compound [Cr].[Ni] VNNRSPGTAMTISX-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- -1 rare earth compound Chemical class 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000005476 soldering Methods 0.000 description 3
- 229910000807 Ga alloy Inorganic materials 0.000 description 2
- 229910001128 Sn alloy Inorganic materials 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 229910000636 Ce alloy Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- SKEYZPJKRDZMJG-UHFFFAOYSA-N cerium copper Chemical compound [Cu].[Ce] SKEYZPJKRDZMJG-UHFFFAOYSA-N 0.000 description 1
- 230000009194 climbing Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001938 differential scanning calorimetry curve Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 229910001325 element alloy Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000011089 mechanical engineering Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000003466 welding Methods 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
- B23K35/302—Cu as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Polishing Bodies And Polishing Tools (AREA)
Abstract
The invention relates to the technical field of superhard abrasive tools, in particular to a multi-element copper-based alloy solder containing rare earth elements, a preparation method and a brazing method thereof, wherein the solder comprises the following components in percentage by weight: 65-70% of copper (Cu), 15-20% of tin (Sn), 8-13% of titanium (Ti), 0-3% of gallium (Ga) and 0-5% of Rare Earth (RE); the microstructure observation of the brazing filler metal and the hardness and shear strength test results of the brazing filler metal show that the addition of the rare earth elements is beneficial to improving the compactness and the mechanical property of the brazing filler metal. In addition, the multi-element copper-based alloy brazing filler metal added with the rare earth elements is used for brazing the diamond, the exposure of the diamond is better, the thermal damage condition of the diamond is lighter, and the service performance of the brazed diamond tool is improved.
Description
Technical Field
The invention relates to the technical field of superhard abrasive tools, in particular to a multi-element copper-based alloy brazing filler metal containing rare earth elements, a preparation method and a brazing method thereof.
Background
Diamond is widely used in the grinding and cutting of glass, ceramics and stone due to its high hardness. Since the synthesis of the first artificial diamond, diamond tools are rapidly popularized and used in the fields of automobile manufacturing, mechanical engineering, national defense and military industry and the like. The manufacture of diamond tools by brazing is one of the main means of manufacturing diamond tools at present. The brazed diamond tool has the advantages of high exposure of diamond particles, good sharpness and the like. Because diamond is chemically inert, research on diamond brazing filler metals is needed. The brazing filler metals currently used for brazing diamond tools mainly comprise silver copper titanium-based (Ag-Cu-Ti), copper tin titanium-based (Cu-Sn-Ti) and nickel chromium-based (Ni-Cr) brazing filler metals. The silver copper titanium base (Ag-Cu-Ti) alloy solder uses titanium (Ti) as an active element to ensure that the solder has higher holding strength to diamond abrasive particles, when the content of the titanium element is too high, the melting point of the solder can be improved, the soldering of the diamond abrasive particles is not facilitated, and meanwhile, the TiC layer can be thickened at the too high soldering temperature, so that the strength of a soldered joint is reduced. In higher temperature working environments, nickel-chromium-based (Ni-Cr) solders are typically used to braze diamond abrasive particles, but the melting point of Ni far exceeds the graphitization temperature of diamond, so it is necessary to add melting point-reducing elements to lower the melting point of the solder. The copper tin titanium base (Cu-Sn-Ti) alloy solder has better wear resistance than silver copper titanium base (Ag-Cu-Ti) alloy solder and lower melting point than nickel chromium base (Ni-Cr) alloy solder, so the copper tin titanium base (Cu-Sn-Ti) alloy solder has wider application. Cu and Ti can form a wear-resistant phase, so that the melting point of the brazing filler metal is reduced, and the wettability of the brazing filler metal is improved. However, when the content of Sn element in the solder is too high, the workability of the solder is adversely affected, and therefore, the components of the solder need to be reasonably mixed.
In view of the above-mentioned drawbacks, the inventors of the present invention have finally obtained the present invention through a long period of research and practice.
Disclosure of Invention
The invention aims to solve the problems of heat damage, low diamond exposure and uneven brazing filler metal structure of the existing brazed diamond, and provides a preparation method of a multi-element copper-based alloy brazing filler metal containing rare earth elements and a brazing method.
In order to realize the purpose, the invention discloses a multi-element copper-based alloy solder containing rare earth elements, which comprises the following components in percentage by mass: 65-70% of copper, 15-20% of tin, 8-13% of titanium, 0-3% of gallium and 0-5% of rare earth.
The invention also discloses a preparation method of the multi-element copper-based alloy solder containing the rare earth elements, which comprises the following steps:
s1: weighing copper, tin, titanium, gallium and rare earth according to the mass percentage, ultrasonically cleaning the copper, tin, titanium, gallium and rare earth in an acetone solution for 10min, then ultrasonically cleaning the copper, tin, titanium, gallium and rare earth in an alcohol solution for 5min, and naturally drying the copper, tin, titanium, gallium and rare earth;
s2: repeatedly smelting the copper and the titanium treated in the step S1 in a vacuum arc furnace for 3-4 times under the condition that the current is 3-5A to obtain a copper-titanium alloy ingot;
s3: and placing the tin, gallium and rare earth processed in the step S1 below the copper-titanium alloy ingot obtained in the step S2, putting the tin, gallium and rare earth together into a vacuum arc furnace, and repeatedly smelting for 3-4 times under the condition that the current is 0.5-2A to obtain the multi-element copper-based alloy brazing filler metal ingot.
In step S1, the purities of copper, tin, titanium, gallium, and rare earth are all 99.5%.
In the step S2, the shielding gas in the solder smelting process is argon gas.
The invention also discloses a brazing method of the multi-element copper-based alloy brazing filler metal containing the rare earth elements, which comprises the following steps:
(1) carrying out suction casting on the multi-element copper-based alloy solder cast ingot into sheet solder with the thickness of 0.5mm by using a suction casting grinding tool;
(2) grinding the surface of the steel substrate by using 240# and 600# sandpaper respectively to remove an oxide layer on the surface of the steel substrate;
(3) putting the steel substrate and the superhard abrasive material treated in the step (2) into an acetone solution and an alcohol solution in sequence for ultrasonic cleaning, and naturally drying;
(4) spreading sheet solder on the upper surface of steel substrate, spreading superhard abrasive on the upper surface of solder layer, brazing in a vacuum brazing furnace with vacuum degree of 1 × 10-3And Pa, keeping the temperature in a vacuum brazing furnace with the brazing temperature of 920 ℃ for 5min, and taking out the brazing sample from the brazing furnace after cooling to the room temperature.
The size of the sheet solder in the step (1) is 15mm multiplied by 6 mm.
The size of the steel matrix in the step (2) is 15mm multiplied by 10mm multiplied by 6 mm.
In the step (3), the ultrasonic cleaning time of the steel matrix and the super-hard abrasive in the acetone solution is 10min, and the cleaning time in the alcohol solution is 5 min.
In the step (3), the heating mode of the vacuum brazing furnace is induction heating, and the heating rate is 10 ℃/min.
The melting point of the brazing filler metal is reduced by adding trace rare earth elements into the copper-based alloy brazing filler metal and forming a low-melting-point rare earth compound with other elements in the brazing filler metal, and the rare earth elements serve as nucleation particles in the solidification process of the liquid brazing filler metal to increase the number of the nucleation particles in the brazing filler metal, so that the purpose of refining grains is achieved.
Compared with the prior art, the invention has the beneficial effects that:
(1) on the basis of the existing multi-element copper-based composite solder, the invention refines the structure of the solder by adding trace rare earth elements, reduces the melting point of the solder, and improves the mechanical property of a soldered joint to improve the service performance of a diamond tool.
(2) According to experimental research, the invention discovers that a compound with a low melting point can be formed in the brazing filler metal by adding trace rare earth elements, and the effect of reducing the melting point of the alloy brazing filler metal is achieved. Too high content of rare earth elements can form high-melting-point compounds in the alloy solder, thereby improving the melting point of the solder and being not beneficial to welding diamond soldered joints. When the mass percentage of the rare earth element in the alloy solder is 0-2%, the effect of reducing the melting point of the alloy solder can be achieved.
(3) The trace rare earth elements added into the brazing filler metal can be eccentrically gathered on the surface of the eutectic structure of the brazing filler metal, so that the surface energy between two phases of the eutectic structure is reduced, the eutectic structure is changed into a rod shape and a spherical shape from a lamellar shape, and the structure of the brazing filler metal is refined. In addition, on one hand, Sn forming eutectic structures in the brazing filler metal is consumed by the compound formed by the rare earth elements; on the other hand, the segregation of the rare earth elements hinders the diffusion of Sn atoms, and the two elements jointly act to reduce the volume fraction of eutectic structures and spheroidize the composition phases of the eutectic structures after the liquid brazing filler metal is solidified.
(4) The multi-element copper-based alloy solder prepared by the invention can reduce the defects of the soldered joint and improve the shear strength of the soldered joint due to the compact structure in the soldering process.
(5) The multi-element alloy solder prepared by the invention has the advantages that the existence of rare earth elements can improve the wettability of the solder, improve the climbing height of carbide on the surface of diamond and increase the wear resistance of a diamond tool.
Drawings
FIG. 1 is a shape diagram of a multi-element copper-based alloy solder ingot;
FIG. 2 is a schematic view of the shape of a suction cast abrasive tool;
FIG. 3 is a microstructure and morphology diagram of a multi-element copper-based alloy solder with 1% of lanthanum (La) added in example 1;
FIG. 4 is a microstructure and morphology diagram of a multi-element copper-based alloy solder with 1% of rare earth cerium (Ce) added in example 2;
FIG. 5 is a microstructure and morphology diagram of a multi-element copper-based alloy solder with 1% of rare earth neodymium (Nd) added in example 1;
FIG. 6 is a microstructure and morphology diagram of a rare earth multi-element copper-based alloy solder not added in comparative example 1;
FIG. 7 is a graph of the shear strength of the braze after the addition of different rare earth elements;
FIG. 8 is a microhardness diagram of the braze after addition of different rare earth elements;
FIG. 9 is a graph of the appearance of a multi-element copper-based alloy solder brazed diamond with 1% of lanthanum (La) added in example 1;
FIG. 10 is a graph of the morphology of a multi-element copper-based alloy solder brazed diamond when 1% rare earth (Ce) was added in example 2;
FIG. 11 is a graph of the appearance of a multi-element brazing filler metal of copper-based alloy brazed diamond in example 3 with 1% of rare earth neodymium (Nd) added;
fig. 12 is a morphology diagram of the multi-element copper-based alloy solder brazed diamond without rare earth in comparative example 1.
FIG. 13 is a DSC chart of comparative example 1 and examples 1, 2, and 3.
Detailed Description
The above and further features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
The metal raw materials involved in the invention are all commercial products, and the purities of the raw materials Cu, Sn, Ti and Ga are 99.5. Rare earth materials used: the mass fraction of lanthanum (La) in the copper-lanthanum alloy (Cu-La) was 10%, the mass fraction of cerium (Ce) in the copper-cerium alloy (Cu-Ce) was 20%, and the purity of neodymium powder was 99.5%.
Example 1
(1) Weighing the following raw materials by using an electronic balance: 5.9g of copper (Cu), 2g of tin (Sn), 1g of titanium (Ti), 0.1g of gallium (Ga) and 1g of copper-lanthanum alloy (Cu-La). Ultrasonically cleaning the weighed raw materials in acetone solution for 10min, then ultrasonically cleaning in alcohol solution for 5min, and naturally drying.
(2) Putting the dried raw materials of copper and titanium into a vacuum electric arc furnace for smelting, wherein the vacuum degree of the vacuum electric arc furnace is kept at 1 x 10-3Pa. In order to prevent the brazing filler metal from being oxidized in the smelting process, argon is flushed into the electric arc furnace as a protective gas. Repeatedly smelting for 3 times under the condition that the current is 3A to obtain the copper-titanium alloy ingot. In order to prevent the volatilization of low-melting-point raw materials, the tin alloy, the gallium alloy and the copper lanthanum alloy are placed below a copper-titanium alloy cast ingot, put into a vacuum arc furnace together, repeatedly smelted for 3 times under the condition that the current is 1A, and taken out of the furnace after natural cooling to obtain the multi-element copper-based alloy solder cast ingot. The shape of the multi-element copper-based alloy ingot is shown in figure 1.
(3) And (4) carrying out suction casting on the smelted alloy cast ingot into a sheet shape by using a suction casting grinding tool. The shape of the suction cast abrasive tool is shown in fig. 2. The cross section of the suction-cast sheet filler metal was polished to a sheet filler metal having a size of 15mm x 6mm and a thickness of 0.5mm using 800# and 600# sandpaper.
(4) A45 # steel block with the size of 15mm multiplied by 10mm multiplied by 6mm is taken, the surface of a steel matrix is polished to be bright by using 240# abrasive paper and 600# abrasive paper respectively, and rust and impurities on the surface of the steel block are removed. And putting the steel block into an acetone solution for ultrasonic cleaning for 10min, then putting the steel block into an alcohol solution for ultrasonic cleaning for 5min, and naturally drying.
(5) Taking the diamond particles with the particle size of 35/40 meshes and good shapes, putting the diamond particles into an acetone solution, carrying out ultrasonic cleaning for 10min, then putting the diamond particles into an alcohol solution, carrying out ultrasonic cleaning for 5min, and naturally drying.
(6) And paving the sheet brazing filler metal on the upper surface of the steel block, paving the diamond particles on the upper surface of the brazing filler metal, putting the brazing filler metal and the diamond particles into a vacuum induction brazing furnace together, keeping the temperature for 5min in a vacuum environment at 920 ℃, and taking out the brazing filler metal after naturally cooling to room temperature to obtain a brazing sample. The vacuum degree of the brazing furnace is kept at 1 x 10 during the brazing process-3The heating mode of the vacuum induction brazing furnace is induction heating, and the heating rate is 10 ℃/min.
Example 2
(1) Weighing the following raw materials by using an electronic balance: 5.9g of copper (Cu), 2g of tin (Sn), 1g of titanium (Ti), 0.1g of gallium (Ga) and 1g of copper-lanthanum alloy (Cu-La). Ultrasonically cleaning the weighed raw materials in acetone solution for 10min, then ultrasonically cleaning in alcohol solution for 5min, and naturally drying.
(2) Putting the dried raw materials of copper and titanium into a vacuum electric arc furnace for smelting, wherein the vacuum degree of the vacuum electric arc furnace is kept at 1 x 10-3Pa. In order to prevent the brazing filler metal from being oxidized in the smelting process, argon is flushed into the electric arc furnace as a protective gas. Repeatedly smelting for 3 times under the condition that the current is 3A to obtain the copper-titanium alloy ingot. In order to prevent the volatilization of low-melting-point raw materials, the tin alloy, the gallium alloy and the copper lanthanum alloy are placed below a copper-titanium alloy cast ingot, put into a vacuum melting furnace together, repeatedly melted for 3 times under the condition that the current is 1A, and taken out of the furnace after natural cooling to obtain the multi-element copper-based alloy brazing filler metal cast ingot. The shape of the multi-element copper-based alloy ingot is shown in figure 1.
(3) And (4) carrying out suction casting on the smelted alloy cast ingot into a sheet shape by using a suction casting grinding tool. The shape of the suction cast abrasive tool is shown in fig. 2. The cross section of the suction-cast sheet filler metal was polished to a sheet filler metal having a size of 15mm x 6mm and a thickness of 0.5mm using 800# and 600# sandpaper.
(4) A45 # steel block with the size of 15mm multiplied by 10mm multiplied by 6mm is taken, the surface of a steel matrix is polished to be bright by using 240# abrasive paper and 600# abrasive paper respectively, and rust and impurities on the surface of the steel block are removed. And putting the steel block into an acetone solution for ultrasonic cleaning for 10min, then putting the steel block into an alcohol solution for ultrasonic cleaning for 5min, and naturally drying.
(5) Taking the diamond particles with the particle size of 35/40 meshes and good shapes, putting the diamond particles into an acetone solution, carrying out ultrasonic cleaning for 10min, then putting the diamond particles into an alcohol solution, carrying out ultrasonic cleaning for 5min, and naturally drying.
(6) And paving the sheet brazing filler metal on the upper surface of the steel block, paving the diamond particles on the upper surface of the brazing filler metal, putting the brazing filler metal and the diamond particles into a vacuum induction brazing furnace together, keeping the temperature for 5min in a vacuum environment at 920 ℃, and taking out the brazing filler metal after naturally cooling to room temperature to obtain a brazing sample. The vacuum degree of the brazing furnace is kept at 1 x 10 during the brazing process-3The heating mode of the vacuum induction brazing furnace is induction heating, and the heating rate is 10 ℃/min.
Example 3
(1) Weighing the following raw materials by using an electronic balance: 6.4g of copper (Cu), 2g of tin (Sn), 1g of titanium (Ti), 0.1g of gallium (Ga), 0.1g of neodymium (Nd). Ultrasonically cleaning the weighed raw materials in acetone solution for 10min, then ultrasonically cleaning in alcohol solution for 5min, and naturally drying.
(2) Putting the dried raw materials of copper and titanium into a vacuum electric arc furnace for smelting, wherein the vacuum degree of the vacuum electric arc furnace is kept at 1 x 10-3Pa. In order to prevent the brazing filler metal from being oxidized in the smelting process, argon is flushed into the electric arc furnace as a protective gas. Repeatedly smelting for 3 times under the condition that the current is 3A to obtain the copper-titanium alloy ingot. In order to prevent the volatilization of the low-melting-point raw materials, tin, gallium and neodymium are placed below a copper-titanium alloy cast ingot, the tin, the gallium and the neodymium are put into a vacuum melting furnace together and repeatedly melted for 3 times under the condition that the current is 1A, and the tin, the gallium and the neodymium are taken out of the furnace after natural cooling to obtain a multi-element copper-based alloy solder cast ingot. The shape of the multi-element copper-based alloy ingot is shown in figure 1.
(3) And (4) carrying out suction casting on the smelted alloy cast ingot into a sheet shape by using a suction casting grinding tool. The shape of the suction cast abrasive tool is shown in fig. 2. The cross section of the suction-cast sheet filler metal was polished to a sheet filler metal having a size of 15mm x 6mm and a thickness of 0.5mm using 800# and 600# sandpaper.
(4) A45 # steel block with the size of 15mm multiplied by 10mm multiplied by 6mm is taken, the surface of a steel matrix is polished to be bright by using 240# abrasive paper and 600# abrasive paper respectively, and rust and impurities on the surface of the steel block are removed. And putting the steel block into an acetone solution for ultrasonic cleaning for 10min, then putting the steel block into an alcohol solution for ultrasonic cleaning for 5min, and naturally drying.
(5) Taking the diamond particles with the particle size of 35/40 meshes and good shapes, putting the diamond particles into an acetone solution, carrying out ultrasonic cleaning for 10min, then putting the diamond particles into an alcohol solution, carrying out ultrasonic cleaning for 5min, and naturally drying.
(6) And paving the sheet brazing filler metal on the upper surface of the steel block, paving the diamond particles on the upper surface of the brazing filler metal, putting the brazing filler metal and the diamond particles into a vacuum induction brazing furnace together, keeping the temperature for 5min in a vacuum environment at 920 ℃, and taking out the brazing filler metal after naturally cooling to room temperature to obtain a brazing sample. The vacuum degree of the brazing furnace is kept at 1 x 10 during the brazing process-3The heating mode of the vacuum induction brazing furnace is induction heating, and the heating rate is 10 ℃/min.
Comparative example 1
(1) Weighing the following raw materials by using an electronic balance: 6.9g of copper (Cu), 2g of tin (Sn), 1g of titanium (Ti) and 0.1g of gallium (Ga). Ultrasonically cleaning the weighed raw materials in acetone solution for 10min, then ultrasonically cleaning in alcohol solution for 5min, and naturally drying.
(2) Putting the dried raw materials of copper and titanium into a vacuum electric arc furnace for smelting, wherein the vacuum degree of the vacuum electric arc furnace is kept at 1 x 10-3Pa. In order to prevent the brazing filler metal from being oxidized in the smelting process, argon is flushed into the electric arc furnace as a protective gas. Repeatedly smelting for 3 times under the condition that the current is 3A to obtain the copper-titanium alloy ingot. In order to prevent the volatilization of the low melting point raw materials, tin and gallium are placed below a copper-titanium alloy cast ingot, are put into a vacuum melting furnace together, are repeatedly melted for 3 times under the condition that the current is 1A, and are taken out of the furnace after being naturally cooled, so that the multi-element copper-based alloy solder cast ingot is obtained. The shape of the multi-element copper-based alloy ingot is shown in figure 1.
(3) And (4) carrying out suction casting on the smelted alloy cast ingot into a sheet shape by using a suction casting grinding tool. The shape of the suction cast abrasive tool is shown in fig. 2. The cross section of the suction-cast sheet filler metal was polished to a sheet filler metal having a size of 15mm x 6mm and a thickness of 0.5mm using 800# and 600# sandpaper.
(4) A45 # steel block with the size of 15mm multiplied by 10mm multiplied by 6mm is taken, the surface of a steel matrix is polished to be bright by using 240# abrasive paper and 600# abrasive paper respectively, and rust and impurities on the surface of the steel block are removed. And putting the steel block into an acetone solution for ultrasonic cleaning for 10min, then putting the steel block into an alcohol solution for ultrasonic cleaning for 5min, and naturally drying.
(5) Taking the diamond particles with the particle size of 35/40 meshes and good shapes, putting the diamond particles into an acetone solution, carrying out ultrasonic cleaning for 10min, then putting the diamond particles into an alcohol solution, carrying out ultrasonic cleaning for 5min, and naturally drying.
(6) And paving the sheet brazing filler metal on the upper surface of the steel block, paving the diamond particles on the upper surface of the brazing filler metal, putting the brazing filler metal and the diamond particles into a vacuum induction brazing furnace together, keeping the temperature for 5min in a vacuum environment at 920 ℃, and taking out the brazing filler metal after naturally cooling to room temperature to obtain a brazing sample. The vacuum degree of the brazing furnace is kept at 1 x 10 during the brazing process-3The heating mode of the vacuum induction brazing furnace is induction heating, and the heating rate is 10 ℃/min.
The performance test of the multi-element copper-based alloy solder obtained in the examples 1-3 and the comparative example is carried out, and the results are as follows:
1. microstructure of brazing filler metal
A metallographic specimen prepared from the multi-element copper-based alloy solder is used for observing the structure and the appearance under a scanning electron microscope. Fig. 3 is a microstructure and morphology diagram of a multi-element copper-based alloy solder with 1% of rare earth lanthanum (La) added in example 1, fig. 4 is a microstructure and morphology diagram of a multi-element copper-based alloy solder with 1% of rare earth cerium (Ce) added in example 2, fig. 5 is a microstructure and morphology diagram of a multi-element copper-based alloy solder with 1% of rare earth neodymium (Nd) added in example 1, and fig. 6 is a microstructure and morphology diagram of a rare earth multi-element copper-based alloy solder without being added in comparative example 1. Observing the graphs in fig. 3-6, it can be found that compared with the solder without adding rare earth elements, the addition of rare earth elements in the multi-element copper-based alloy solder can refine the solder structure, the microstructure of the surface eutectic structure is micro-morphology, and the defects in the solder structure are obviously reduced, which is beneficial to improving the mechanical property of the soldered joint. Meanwhile, the influence of different kinds of rare earth elements on the microstructure of the alloy solder is different.
2. Shear strength of brazing filler metal
Fig. 7 shows the shear strength of the solder after adding different rare earth elements, and it can be seen that the shear strength of the solder can be improved by adding different rare earth elements into the multi-element copper-based alloy solder, and the shear strength of the alloy solder added with the rare earth element neodymium (Nd) is the highest, and the shear strength of the solder is improved from 244MPa to 309MPa, which is consistent with the structural properties of the solder.
3. Microhardness of solder
Fig. 8 shows the microhardness of the solder after different rare earth elements are added, and it can be seen from fig. 8 that different kinds of rare earth elements can improve the microhardness of the solder, and the microhardness of the alloy solder added with the rare earth element neodymium (Nd) is the highest, and the microhardness of the alloy solder is improved from 232HV to 265 HV.
4. Micro-topography of diamond braze joints
FIG. 9 is a graph of the appearance of a multi-element copper-based alloy solder brazed diamond with 1% of lanthanum (La) added in example 1; FIG. 10 is a graph of the morphology of a multi-element copper-based alloy solder brazed diamond when 1% rare earth (Ce) was added in example 2; FIG. 11 is a graph of the appearance of a multi-element brazing filler metal of copper-based alloy brazed diamond in example 3 with 1% of rare earth neodymium (Nd) added; fig. 12 is a morphology diagram of the multi-element copper-based alloy solder brazed diamond without rare earth in comparative example 1. From the topography of the brazed diamond it can be seen that: the brazing diamond to which no rare earth element is added is more seriously burned out and the exposure of the diamond is low, which may adversely affect the use properties of the brazing diamond tool. The brazing diamond added with the rare earth elements has better appearance, wherein the brazing filler metal added with the rare earth neodymium has the best appearance, and the defects of the brazing filler metal are the least.
5. DSC curve of alloy solder
FIG. 13 is a DSC chart of comparative example 1 and examples 1, 2, and 3. The peak of the curve is taken as the melting temperature of the solder. It can be seen from the data in the figure that the melting temperature of the copper-based alloy solder without addition of the rare earth element is 875.6 deg.c. The melting point of the solder is reduced after the rare earth element is added, and particularly the melting point of the solder is reduced by 14.1 ℃ after the rare earth element La is added. This is because the rare earth element forms a low melting point rare earth compound with Cu and Sn in the brazing filler metal after adding the rare earth element in the copper-based brazing filler metal, and the melting point of the brazing filler metal is lowered. Because the melting points of the rare earth compounds formed by different rare earths are different, the influence of different rare earth elements on the melting point of the copper-based alloy solder is different.
In conclusion, the multi-element copper-based alloy solder containing the rare earth elements improves the microstructure of the copper-based alloy solder by adding the rare earth elements, improves the shearing strength and hardness of the solder and improves the service performance of a brazed diamond tool.
The foregoing is merely a preferred embodiment of the invention, which is intended to be illustrative and not limiting. It will be understood by those skilled in the art that various changes, modifications and equivalents may be made therein without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. The multi-element copper-based alloy brazing filler metal containing rare earth elements is characterized by comprising the following components in percentage by mass: 65-70% of copper, 15-20% of tin, 8-13% of titanium, 0-3% of gallium and 0-5% of rare earth.
2. A method for preparing a brazing filler metal for multi-element copper-based alloys containing rare earth elements according to claim 1, comprising the steps of:
s1: weighing copper, tin, titanium, gallium and rare earth according to the mass percentage, ultrasonically cleaning the copper, tin, titanium, gallium and rare earth in an acetone solution for 10min, then ultrasonically cleaning the copper, tin, titanium, gallium and rare earth in an alcohol solution for 5min, and naturally drying the copper, tin, titanium, gallium and rare earth;
s2: smelting the copper and the titanium treated in the step S1 in a vacuum arc furnace for 3-4 times under the condition that the current is 3-5A to obtain a copper-titanium alloy ingot;
s3: and placing the tin, gallium and rare earth processed in the step S1 below the copper-titanium alloy ingot obtained in the step S2, putting the tin, gallium and rare earth together into a vacuum arc furnace, and smelting for 3-4 times under the condition that the current is 0.5-2A to obtain the multi-element copper-based alloy brazing filler metal ingot.
3. The method for preparing a multi-element copper-based alloy solder containing rare earth elements according to claim 2, wherein the purities of copper, tin, titanium, gallium and rare earth elements in step S1 are all 99.5%.
4. The method for preparing a multi-element copper-based alloy solder containing rare earth elements according to claim 2, wherein in the step S2, the protective gas in the solder smelting process is argon.
5. A brazing method for a brazing filler metal of a multi-element copper-based alloy containing a rare earth element according to claim 1, comprising the steps of:
(1) carrying out suction casting on the multi-element copper-based alloy solder cast ingot into sheet solder with the thickness of 0.5mm by using a suction casting grinding tool;
(2) grinding the surface of the steel substrate by using 240# and 600# sandpaper respectively to remove an oxide layer on the surface of the steel substrate;
(3) putting the steel substrate and the superhard abrasive material treated in the step (2) into an acetone solution and an alcohol solution in sequence for ultrasonic cleaning, and naturally drying;
(4) spreading sheet solder on the upper surface of steel substrate, spreading superhard abrasive on the upper surface of solder layer, brazing in a vacuum brazing furnace with vacuum degree of 1 × 10-3And Pa, keeping the temperature in a vacuum brazing furnace with the brazing temperature of 920 ℃ for 5min, and taking out the brazing sample from the brazing furnace after cooling to the room temperature.
6. The brazing method for a brazing filler metal of a multi-element copper-based alloy containing a rare earth element according to claim 5, wherein the size of the brazing filler metal sheet in the step (1) is 15mm x 6 mm.
7. The brazing method for a brazing filler metal of a multi-element copper-based alloy containing a rare earth element according to claim 5, wherein the size of the steel matrix in said step (2) is 15mm x 10mm x 6 mm.
8. The brazing method for the brazing filler metal of the multi-element copper-based alloy containing the rare earth element according to claim 5, wherein in the step (3), the steel substrate and the superabrasive are ultrasonically cleaned in the acetone solution for 10min, and cleaned in the alcohol solution for 5 min.
9. The brazing method of a brazing filler metal of a multi-element copper-based alloy containing a rare earth element according to claim 5, wherein in the step (3), the heating manner of the vacuum brazing furnace is induction heating, and the temperature rise rate is 10 ℃/min.
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