Method for rapidly preparing silver-copper-titanium foil strip brazing filler metal

Abstract

The invention discloses a method for rapidly preparing silver-copper-titanium foil strip brazing filler metal, and belongs to the technical field of active brazing filler metal. The preparation method comprises the following steps: (1) uniformly mixing silver-copper alloy powder and titanium powder or titanium hydride powder, pressing into a block blank, and sintering to obtain a silver-copper-titanium block blank or a silver-copper titanium hydride block blank; (2) the block blank is subjected to multi-group cold rolling and intermediate annealing circulation treatment till the thickness meets the requirement, and plate strip brazing filler metal is obtained; and (3) carrying out vacuum annealing and cold rolling on the plate strip brazing filler metal to obtain the finished product silver-copper-titanium foil strip brazing filler metal. The preparation method is optimally designed, generation of copper-titanium compounds is effectively inhibited, the types and forms of the copper-titanium compounds are regulated and controlled, the machinability and activity of the brazing filler metal are guaranteed, the preparation period of the brazing filler metal is remarkably shortened, and high-efficiency and high-quality preparation of the foil strip brazing filler metal with the high titanium content is achieved.

Description

Technical Field

[0001] This invention belongs to the field of active solder technology, and specifically relates to a method for rapidly preparing silver-copper-titanium foil solder. Background Technology

[0002] Silver-copper-titanium solders are currently the most widely used active solders, playing an indispensable role in high-end technology fields such as power electronic packaging, aerospace, and precision manufacturing. Currently, silver-copper-titanium solder foils are the most widely used due to their high density, good compositional uniformity, and wide applicability in product forms. The preparation methods for silver-copper-titanium foils can be divided into smelting, multilayer composite, and powder metallurgy. However, regardless of the method used, titanium inevitably reacts with copper to form brittle copper-titanium compounds (especially Ti₂Cu, CuTi, and Cu₂Ti). This reaction is particularly pronounced when the titanium content in the silver-copper-titanium solder foil is high, leading to a decrease in the solder's activity and plasticity.

[0003] Among existing preparation methods, powder metallurgy has the advantages of achieving microstructure control, processing feasibility, and high yield, making it more widely applicable.

[0004] Existing technology (CN114227064A) discloses a method for preparing silver-copper-titanium layered composite strips through layered assembly, vacuum brazing, and rolling. However, it suffers from problems such as high requirements for the composite contact interface and asynchronous deformation between materials with different physical properties leading to easy delamination during rolling. Existing technology (CN114921680A) discloses a method for preparing strip-shaped silver-copper-titanium brazing filler metal: powder mixing, compact pressing, vacuum hot pressing sintering, and cold rolling / vacuum annealing. However, it suffers from problems such as a long preparation process, complex equipment, and low yield of brazing filler metal with high titanium content (≥4wt%). Existing technology (CN106521) 203A) discloses a method for preparing silver-copper-titanium alloy foil strip: wet ball milling-cold isostatic pressing-vacuum pre-sintering-hot isostatic pressing-rolling. However, it has problems such as long preparation process and complex equipment. The prior art (CN113976877A) discloses a method for preparing solder sheets using silver-copper-titanium solder paste. However, it has problems such as limited solder sheet size or complex process and long time consumption. The prior art (CN116652452B) discloses obtaining brazing filler metal by electroplating silver and copper on titanium foil and then performing vacuum diffusion treatment. However, it has problems such as difficulty in controlling the plating thickness, easy formation of internal defects, complex process and long time consumption.

[0005] Therefore, it is necessary to provide a method for rapidly preparing silver-copper-titanium foil-strip solder, which can effectively improve the performance of the foil-strip solder while achieving short-cycle and high-efficiency preparation. Summary of the Invention

[0006] To overcome the problems in the prior art, this invention optimizes the preparation method and leverages the overall synergistic effect of the preparation method to achieve short-cycle, high-efficiency, and high-quality preparation of high-titanium content foil-strip solder.

[0007] To achieve the above objectives, the present invention is implemented through the following technical solution: This invention proposes a method for rapidly preparing silver-copper-titanium foil solder, the method comprising the following steps: (1) Mix silver-copper alloy powder and titanium powder or titanium hydride powder, press into a block and sinter to obtain silver-copper titanium block or silver-copper titanium hydride block.

[0008] (2) The blank is subjected to multiple cold rolling and intermediate annealing cycles until the thickness meets the requirements to obtain the strip brazing filler metal.

[0009] The thickness of the solder strip obtained in this step should be 3 to 7 times that of the finished foil solder strip.

[0010] In this step, the specific process of multiple cold rolling and intermediate annealing cycles is as follows: first, the billet is cold rolled; after the cold rolling is completed, intermediate annealing is performed; then, cold rolling is performed again; then, intermediate annealing is performed again, and so on, until the final cold rolling is completed and the brazing filler metal meets the thickness requirements. After the final cold rolling, intermediate annealing is no longer performed.

[0011] (3) Vacuum annealing and cold rolling of the strip brazing filler metal into finished silver-copper-titanium foil brazing filler metal.

[0012] Preferably, in step (1), the silver-copper alloy powder has a particle size ≤100μm and a D50 of 38~53μm; the titanium powder or hydride titanium powder has a particle size of 5~25μm and a sphericity ≥0.9.

[0013] Preferably, the sintering in step (1) and the intermediate annealing in step (2) are both carried out under flux protection.

[0014] Preferably, the flux is at least one of QJ101 and QJ102.

[0015] When the flux is a mixture of QJ101 and QJ102, the two substances are mixed in any proportion.

[0016] Preferably, in step (1), the sintering process of the silver-copper-titanium billet is as follows: first, the silver-copper-titanium billet is placed in flux at 350~400℃ and kept at that temperature for 5~10 minutes, then heated to 780~800℃ at a rate of ≥8℃ / min and kept at that temperature for 5~15 minutes, and then directly water-cooled to room temperature.

[0017] Preferably, in step (1), the sintering process of the silver-copper titanium hydride billet is as follows: first, the silver-copper titanium hydride billet is placed in flux at 300~350℃ and kept at that temperature for 5~10 minutes, then the temperature is increased to 650~700℃ at a rate of 4~8℃ / min, and then increased to 780~800℃ at a rate of ≥8℃ / min and kept at that temperature for 5~15 minutes before being directly water-cooled to room temperature.

[0018] Preferably, in step (2), the intermediate annealing process is as follows: the brazing filler metal is placed in flux at 650~680℃ and kept at 3~10 minutes or heated to 720~740℃ with a flame under flux protection, and then directly cooled to room temperature with water, and the number of intermediate annealing times is ≤6.

[0019] Preferably, in step (3), the vacuum annealing process is performed with a vacuum degree ≤ 1.0 × 10⁻⁶. -3 Pa is held at 640~670℃ for 3~10min and then cooled to below 250℃ at a rate of ≥8℃ / min, with the number of vacuum annealing cycles ≤2.

[0020] Preferably, the finished silver-copper-titanium foil brazing filler metal has a thickness of 0.05~0.12mm and a titanium content of 3~8wt%.

[0021] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. This invention, through the synergistic effect of sintering and annealing processes, inhibits the formation and growth of brittle copper-titanium compounds, regulates the types of compounds, suppresses the nucleation and growth of Cu4Ti, avoids the formation of Ti2Cu, CuTi, etc., and promotes the compounds to be dispersed in the matrix in the form of fine particles, generating only finely dispersed Cu4Ti phase, reducing the consumption of active Ti, thereby effectively improving the activity of silver-copper-titanium foil solder.

[0022] 2. Compared with foil-strip brazing filler metal prepared by conventional methods, the present invention optimizes the preparation method and gives full play to the synergistic effect of sintering, annealing and rolling, which effectively improves the plasticity of silver-copper-titanium foil-strip brazing filler metal and can increase the elongation by 10%~30%.

[0023] 3. The present invention uses flux protection to synergize annealing and sintering conditions, which reduces the time for a single vacuum sintering or annealing from several hours or tens of hours to less than 20 minutes, and shortens the overall preparation time by 50% to 80%.

[0024] 4. Under normal circumstances, the preparation of high titanium content silver-copper-titanium solders will face abnormal nucleation and growth of Ti2Cu, CuTi, etc., forming large block or continuous network structures, which makes it difficult to control the microstructure, resulting in poor solder plasticity, and a large consumption of Ti, which deteriorates the solder's processability and activity. The method of the present invention can prepare high-activity, high-plasticity high titanium content foil strip solders. Attached Figure Description

[0025] Figure 1 The images show actual photos of the silver-copper-titanium foil brazing filler prepared in Examples 1 and 2 of this invention.

[0026] Figure 2 The image shows a scanning electron microscope (SEM) image of the microstructure of the silver-copper-titanium foil brazing filler metal prepared in Example 1. Detailed Implementation

[0027] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0028] Example 1: In this embodiment, AgCu26.7Ti4.5 foil solder with a thickness of 0.1 mm was prepared using the following method: (1) Weigh 2.0 kg of AgCu28 powder with a particle size of -160 mesh (≤96μm) and D50 of 53μm and titanium hydride powder with a particle size of 5~25μm according to the theoretical mass ratio. After mixing the AgCu28 powder and titanium hydride powder, press them into silver-copper titanium hydride blocks with a thickness of 8mm by cold isostatic pressing.

[0029] (2) Place the billet directly into QJ102 at 350℃ and keep it at that temperature for 10 minutes. Then, raise the temperature to 680℃ at a rate of 4℃ / min, raise it to 800℃ at a rate of 8℃ / min and keep it at that temperature for 15 minutes. Then, cool it directly to room temperature with water.

[0030] (3) The billet is rolled to a thickness of 7.2 mm using a twin-roll mill and then placed in a QJ102 at 680℃ for 10 min and then directly water-cooled. Then it is rolled to a thickness of 6.0 mm and placed in a QJ102 at 680℃ for 10 min and then directly water-cooled. Then it is rolled to a thickness of 4.5 mm and placed in a QJ102 at 680℃ for 10 min and then directly water-cooled. Then it is rolled to a thickness of 3.0 mm and placed in a QJ102 at 680℃ for 10 min and then directly water-cooled. Then it is rolled to a thickness of 1.8 mm and placed in a QJ102 at 660℃ for 10 min and then directly water-cooled. Then it is rolled to a thickness of 1.0 mm and placed in a QJ102 at 660℃ for 5 min and then directly water-cooled. Finally, it is rolled to a thickness of 0.4 mm.

[0031] (4) Place the foil strip brazing blank into a vacuum furnace and evacuate it to 1.0 × 10⁻⁶. -3 Below Pa, after holding at 650℃ for 10 minutes, the temperature is reduced to room temperature at a rate of 8℃ / min.

[0032] (5) The foil strip brazing blank is rolled to 0.1 mm using a four-roll mill, and the cracked edge is removed to obtain the finished foil strip.

[0033] The microstructure of the finished silver-copper-titanium foil solder prepared in this embodiment is as follows: Figure 2 As shown, Figure 2In the image, the gray area represents the Ag-Cu alloy matrix, and the black area represents the second phase formed by Cu4Ti compounds and elemental Ti. Figure 2 It can be seen that the second phase is dispersed in the matrix as fine particles, and no Ti2Cu, CuTi, or other phases were observed. This proves that the method of the present invention can effectively suppress the formation and growth of brittle copper-titanium compounds, control the types of compounds, suppress the nucleation and growth of Cu4Ti, and avoid the formation of Ti2Cu, CuTi, etc., thereby improving the plasticity and activity of the silver-copper-titanium foil solder prepared by the present invention.

[0034] Comparative Example 1 This comparative example uses the same method as Example 1 to prepare silver-copper-titanium foil brazing filler metal, the difference being that step (2) in this comparative example is replaced by placing the blank directly into QJ102 at 800℃ for 25 minutes.

[0035] In the brazing filler metal prepared in this comparative example, compounds such as Cu4Ti, CuTi, and Ti2Cu were generated, and some of these compounds grew into lumps, reducing the plasticity and activity of the brazing filler metal. This resulted in edge cracking of the foil brazing filler metal and a 5% reduction in yield.

[0036] Compared with Example 1, it can be seen that directly using a higher temperature for a longer sintering time will lead to the growth of copper-titanium compounds and the formation of various brittle compounds, further consuming Ti, affecting the activity of the solder and reducing its plasticity.

[0037] Comparative Example 2 This comparative example uses the same method as Example 1 to prepare silver-copper-titanium foil solder, except that the flux protection annealing in step (3) is replaced with high vacuum annealing.

[0038] The Cu4Ti compound in the solder prepared in this embodiment has an increased size and a small amount of extremely brittle CuTi compounds are formed. This not only reduces the plasticity and activity of the solder, but also increases the preparation time by 60%. At the same time, the wetting angle of the silver-copper-titanium foil solder prepared in this comparative example on alumina ceramic is 12°, while the wetting angle of the silver-copper-titanium foil solder prepared in Example 1 is 10°. Therefore, using flux-protected annealing, compared with high vacuum annealing, can not only effectively improve the plasticity, activity and wetting performance of the solder, but also effectively and significantly reduce the preparation cycle.

[0039] Comparative Example 3 This comparative example uses the same method as Example 1 to prepare silver-copper-titanium foil brazing filler metal, except that the cooling method in step (4) is changed to furnace cooling (cooling rate is about 4°C / min).

[0040] The Cu4Ti compound in the brazing filler metal prepared in this comparative example has an increased size, which consumes more active Ti, resulting in a decrease in the plasticity and activity of the brazing filler metal.

[0041] Compared with Example 1, it can be seen that the size of the compound can be adjusted by controlling the cooling rate, thereby controlling the solder performance.

[0042] Comparative Example 4 This comparative example uses the same method as Example 1 to prepare silver-copper-titanium foil solder, except that step (4) is replaced with flux-protected annealing.

[0043] The thin solder thickness in this comparative example increases the difficulty of flux protection annealing, which in turn increases the difficulty of solder quality control and consequently increases the preparation time.

[0044] Comparative Example 5 The comparative example uses the same method as Example 1 to prepare silver-copper-titanium foil strip brazing filler metal, the difference being that: in step (3), the brazing filler metal is annealed once when rolled to 7.5mm, 6.8mm, 5.4mm, 4.0mm, 2.8mm, 1.8mm and 0.9mm respectively, that is, the number of annealing times is increased from 6 times to 7 times.

[0045] Compared with Example 1, it can be seen that the annealing time in this comparative example is longer due to the increase in the number of intermediate annealing cycles, which in turn leads to an increase in the size of the Cu4Ti compound and an increase in the preparation time.

[0046] Example 2: In this embodiment, AgCu26.5Ti5.5 foil solder with a thickness of 0.1 mm was prepared using the following method: (1) Weigh 1.5 kg of AgCu28 powder with a particle size of -160 mesh (≤96μm) and D50 of 38μm and titanium hydride powder with a particle size of 5~25μm according to the theoretical mass ratio. After mixing the AgCu28 powder and titanium hydride powder, press them into silver-copper titanium hydride blocks with a thickness of 6mm by cold isostatic pressing.

[0047] (2) Place the billet directly into QJ101 at 350℃ and keep it at that temperature for 10 minutes. Then, raise the temperature to 700℃ at a rate of 4℃ / min, raise it to 800℃ at a rate of 10℃ / min and keep it at that temperature for 10 minutes. Then, cool it directly to room temperature with water.

[0048] (3) The billet is rolled to 5.4 mm using a twin-roll mill. QJ101 is applied to the surface of the brazing filler metal and heated to 740°C with a flame. Then it is directly cooled to room temperature with water. The billet is then rolled to 4.5 mm thick. QJ101 is applied to the surface of the brazing filler metal and heated to 740°C with a flame. Then it is directly cooled to room temperature with water. The billet is then rolled to 3.0 mm thick. QJ101 is applied to the surface of the brazing filler metal and heated to 740°C with a flame. Then it is directly cooled to room temperature with water. The billet is then rolled to 1.8 mm thick. QJ101 is applied to the surface of the brazing filler metal and heated to 730°C with a flame. Then it is directly cooled to room temperature with water. The billet is then rolled to 1.0 mm thick. QJ101 is applied to the surface of the brazing filler metal and heated to 720°C with a flame. Then it is directly cooled to room temperature with water. Finally, the billet is rolled to 0.4 mm thick.

[0049] (4) Place the foil strip brazing blank into a vacuum furnace and evacuate it to 1.0 × 10⁻⁶. -3 Below Pa, after holding at 670℃ for 10 minutes, the temperature is reduced to room temperature at a rate of 9℃ / min.

[0050] (5) The foil strip brazing blank is rolled to 0.1 mm using a four-roll mill, and the cracked edge is removed to obtain the finished foil strip brazing blank.

[0051] Comparative Example 6 The finished foil solder was prepared using the same method as in Example 2. The difference is that in this comparative example, steps (2) and (3) were carried out under vacuum conditions.

[0052] Compared with Comparative Example 6, Example 2 reduced the total preparation time by 65%.

[0053] Example 3: In this embodiment, AgCu26.7Ti4.5 foil solder with a thickness of 0.05 mm was prepared using the following method: (1) Weigh 2.0 kg of AgCu28 powder with a particle size of -160 mesh (≤96μm) and D50 of 38μm and titanium powder with a particle size of 5~25μm and a sphericity of 0.92 according to the theoretical mass ratio. After mixing the AgCu28 powder and titanium powder, press them into silver-copper-titanium ingots with a thickness of 8 mm by cold isostatic pressing.

[0054] (2) Place the billet directly into QJ102 at 400℃ and keep it warm for 5 minutes. Then, raise the temperature to 780℃ at a rate of 8℃ / min and keep it warm for 15 minutes before directly water cooling to room temperature.

[0055] The material was rolled to a thickness of 7.2 mm using a twin-roll mill, then placed in a QJ102 at 650℃ for 10 minutes and directly water-cooled. It was then rolled to a thickness of 6.0 mm and placed in a QJ102 at 650℃ for 10 minutes, followed by direct water cooling. Next, it was rolled to a thickness of 4.5 mm and placed in a QJ102 at 680℃ for 10 minutes, followed by direct water cooling. It was then rolled to a thickness of 3.0 mm and placed in a QJ102 at 650℃ for 10 minutes, followed by direct water cooling. It was then rolled to a thickness of 1.8 mm and placed in a QJ102 at 650℃ for 10 minutes, followed by direct water cooling. It was then rolled to a thickness of 1.0 mm and placed in a QJ102 at 650℃ for 10 minutes, followed by direct water cooling. Finally, it was rolled to a thickness of 0.4 mm.

[0056] (4) Place the foil strip brazing blank into a vacuum furnace and evacuate it to 1.0 × 10⁻⁶. -3 Below Pa, the filler metal was held at 640℃ for 10 min, then cooled to room temperature at a rate of 8℃ / min. The filler metal was then rolled to 0.12 mm using a four-roll mill, and finally placed in a vacuum furnace and evacuated to a vacuum level of 1.0 × 10⁻⁶. -3 Below Pa, after holding at 640℃ for 10 min, the temperature is lowered to room temperature at 8℃ / min. Then, the brazing filler metal is rolled to 0.05 mm using a four-roll mill. Finally, the fission is removed to obtain the finished silver-copper-titanium foil brazing filler metal.

[0057] Compared with the method of using a high vacuum atmosphere throughout the process (including vacuum sintering and vacuum annealing), the preparation time of this embodiment is shortened by 54%.

[0058] Example 4 In this embodiment, AgCu25.7Ti8 foil solder with a thickness of 0.1 mm was prepared using the following method: (1) Weigh 1.6 kg of AgCu28 powder with a particle size of 5~25 μm and D50 of 45 μm and titanium hydride powder with a particle size of -160 mesh (≤96 μm) according to the theoretical mass ratio. After mixing the AgCu28 powder and titanium hydride powder, press them into silver-copper titanium hydride blocks with a thickness of 6 mm by cold isostatic pressing.

[0059] (2) Place the billet directly into a mixture of QJ101 and QJ102 at 330℃ and keep it at that temperature for 7 minutes. Then, raise the temperature to 650℃ at a rate of 6℃ / min, raise it to 780℃ at a rate of 9℃ / min and keep it at that temperature for 5 minutes before directly water cooling it to room temperature.

[0060] (3) The billet is rolled to a thickness of 5.4 mm using a twin-roll mill and then placed in a mixture of QJ101 and QJ102 at 670℃ for 8 minutes and then directly water-cooled. Then it is rolled to a thickness of 4.5 mm and placed in a mixture of QJ101 and QJ102 at 660℃ for 5 minutes and then directly water-cooled. Then it is rolled to a thickness of 3.2 mm and placed in a mixture of QJ101 and QJ102 at 660℃ for 5 minutes and then directly water-cooled. Then it is rolled to a thickness of 2.0 mm and placed in a mixture of QJ101 and QJ102 at 650℃ for 5 minutes and then directly water-cooled. Then it is rolled to a thickness of 1.0 mm and placed in a mixture of QJ101 and QJ102 at 650℃ for 5 minutes and then directly water-cooled. Finally, it is rolled to a thickness of 0.4 mm.

[0061] (4) Place the foil strip brazing blank into a vacuum furnace and evacuate it to 1.0 × 10⁻⁶. -3 Below Pa, after holding at 650℃ for 3 minutes, the temperature is reduced to room temperature at a rate of 10℃ / min.

[0062] (5) The foil strip brazing blank is rolled to 0.1 mm using a four-roll mill, and the cracked edge is removed to obtain the finished foil strip.

[0063] The properties of the finished silver-copper-titanium foil brazing filler metal prepared in this embodiment are similar to those in Example 1.

[0064] Example 5 In this embodiment, AgCu26.7Ti4.5 foil solder with a thickness of 0.1 mm was prepared using the following method: (1) Weigh 2.0 kg of AgCu28 powder with a particle size of -160 mesh (≤96μm) and D50 of 53μm and titanium hydride powder with a particle size of 5~25μm according to the theoretical mass ratio. After mixing the AgCu28 powder and titanium hydride powder, press them into silver-copper titanium hydride blocks with a thickness of 8mm by cold isostatic pressing.

[0065] (2) Place the billet directly into QJ102 at 300℃ and keep it at that temperature for 5 minutes. Then, raise the temperature to 700℃ at a rate of 8℃ / min, and then raise the temperature to 790℃ at a rate of 10℃ / min and keep it at that temperature for 15 minutes before directly cooling it to room temperature with water.

[0066] (3) The billet is rolled to a thickness of 7.2 mm using a twin-roll mill and then placed in a QJ102 at 680℃ for 9 min and then directly water-cooled. Then it is rolled to a thickness of 6.0 mm and placed in a QJ102 at 680℃ for 8 min and then directly water-cooled. Next, it is rolled to a thickness of 4.5 mm and placed in a QJ102 at 680℃ for 7 min and then directly water-cooled. Then it is rolled to a thickness of 3.0 mm and placed in a QJ102 at 680℃ for 6 min and then directly water-cooled. Then it is rolled to a thickness of 1.8 mm and placed in a QJ102 at 680℃ for 5 min and then directly water-cooled. Then it is rolled to a thickness of 1.0 mm and placed in a QJ102 at 680℃ for 3 min and then directly water-cooled. Finally, it is rolled to a thickness of 0.5 mm.

[0067] (4) Place the foil strip brazing blank into a vacuum furnace and evacuate it to 1.0 × 10⁻⁶. -3 Below Pa, after holding at 670℃ for 7 minutes, the temperature is reduced to room temperature at a rate of 8℃ / min.

[0068] (5) The foil strip brazing blank is rolled to 0.1 mm using a four-roll mill, and the cracked edge is removed to obtain the finished foil strip.

[0069] The properties of the finished silver-copper-titanium foil brazing filler metal prepared in this embodiment are similar to those in Example 1.

[0070] Example 6 In this embodiment, AgCu25.7Ti8 foil solder with a thickness of 0.05 mm was prepared using the following method: (1) Weigh 2.0 kg of AgCu28 powder with a particle size of -160 mesh (≤96μm) and D50 of 38μm and titanium powder with a particle size of 5~25μm and a sphericity of 0.92 according to the theoretical mass ratio. After mixing the AgCu28 powder and titanium powder, press them into silver-copper-titanium ingots with a thickness of 8 mm by cold isostatic pressing.

[0071] (2) Place the billet directly into QJ102 at 350℃ and keep it warm for 10 minutes. Then, raise the temperature to 800℃ at a rate of 9℃ / min and keep it warm for 5 minutes before directly water cooling to room temperature.

[0072] The material was rolled to a thickness of 7.2 mm using a twin-roll mill, then placed in a QJ102 at 680℃ for 10 minutes and directly water-cooled. It was then rolled to a thickness of 6.0 mm and placed in a QJ102 at 680℃ for 10 minutes and directly water-cooled. Next, it was rolled to a thickness of 4.5 mm and placed in a QJ102 at 680℃ for 10 minutes and directly water-cooled. It was then rolled to a thickness of 3.0 mm and placed in a QJ102 at 680℃ for 10 minutes and directly water-cooled. It was then rolled to a thickness of 1.8 mm and placed in a QJ102 at 670℃ for 10 minutes and directly water-cooled. It was then rolled to a thickness of 1.0 mm and placed in a QJ102 at 660℃ for 10 minutes and directly water-cooled. Finally, it was rolled to a thickness of 0.4 mm.

[0073] (4) Place the foil strip brazing blank into a vacuum furnace and evacuate it to 1.0 × 10⁻⁶. -3 Below Pa, after holding at 650℃ for 10 min, the filler metal is cooled to room temperature at a rate of 8℃ / min. The filler metal is then rolled to 0.12 mm using a four-roll mill. Finally, the filler metal is placed in a vacuum furnace and evacuated to a vacuum level of 1.0 × 10⁻⁶. -3 Below Pa, after holding at 640℃ for 8 minutes, the temperature is lowered to room temperature at 8℃ / min. Then, the brazing filler metal is rolled to 0.05mm using a four-roll mill. Finally, the fission is removed to obtain the finished silver-copper-titanium foil brazing filler metal.

[0074] The properties of the finished silver-copper-titanium foil strip brazing filler metal prepared in this embodiment are similar to those in Example 3.

[0075] Example 7 In this embodiment, AgCu26.7Ti4.5 foil solder with a thickness of 0.05 mm was prepared using the following method: (1) Weigh 2.0 kg of AgCu28 powder with a particle size of 5~25 μm and a sphericity of 0.95 and a particle size of -160 mesh (≤96 μm) and D50 of 38 μm, and titanium powder with a particle size of 5~25 μm and a sphericity of 0.95 according to the theoretical mass ratio. After mixing the AgCu28 powder and titanium powder, press them into silver-copper-titanium ingots with a thickness of 8 mm by cold isostatic pressing.

[0076] (2) Place the billet directly into QJ102 at 380℃ and keep it at that temperature for 7 minutes. Then, raise the temperature to 790℃ at a rate of 10℃ / min and keep it at that temperature for 15 minutes before directly cooling it to room temperature with water.

[0077] The material was rolled to a thickness of 7.2 mm using a twin-roll mill, then placed in a QJ102 at 680℃ for 10 minutes and directly water-cooled. It was then rolled to a thickness of 6.0 mm and placed in a QJ102 at 680℃ for 10 minutes, followed by direct water cooling. Next, it was rolled to a thickness of 4.5 mm and placed in a QJ102 at 680℃ for 10 minutes, followed by direct water cooling. It was then rolled to a thickness of 3.0 mm and placed in a QJ102 at 680℃ for 10 minutes, followed by direct water cooling. It was then rolled to a thickness of 1.8 mm and placed in a QJ102 at 660℃ for 10 minutes, followed by direct water cooling. It was then rolled to a thickness of 1.0 mm and placed in a QJ102 at 660℃ for 10 minutes, followed by direct water cooling. Finally, it was rolled to a thickness of 0.4 mm.

[0078] (4) Place the foil strip brazing blank into a vacuum furnace and evacuate it to 1.0 × 10⁻⁶. -3 Below Pa, after holding at 670℃ for 7 minutes, the filler metal was cooled to room temperature at a rate of 8℃ / min. The filler metal was then rolled to 0.12 mm using a four-roll mill. Finally, the filler metal was placed in a vacuum furnace and evacuated to a vacuum level of 1.0 × 10⁻⁶. -3Below Pa, after holding at 670℃ for 10 minutes, the temperature is lowered to room temperature at 8℃ / min. Then, the brazing filler metal is rolled to 0.05mm using a four-roll mill. Finally, the fission is removed to obtain the finished silver-copper-titanium foil brazing filler metal.

[0079] The properties of the finished silver-copper-titanium foil strip brazing filler metal prepared in this embodiment are similar to those in Example 3.

[0080] In summary, this invention optimizes the preparation method of silver-copper-titanium foil strip solder, effectively improving the solder's plasticity, activity, wettability, and other properties, while significantly shortening the solder preparation cycle, thus achieving efficient and high-quality preparation of silver-copper-titanium foil strip solder.

[0081] Finally, it should be noted that although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for rapidly preparing a silver-copper-titanium foil ribbon solder, characterized by, The preparation method specifically comprises the following steps: (1) uniformly mixing silver copper alloy powder and titanium powder or titanium hydride powder, pressing into a compact and sintering to obtain a silver copper titanium compact or a silver copper titanium hydride compact; (2) performing multiple cold rolling and intermediate annealing cycle treatment on the compact until the thickness reaches the requirement to obtain a plate strip solder; (3) vacuum annealing the plate strip solder and cold rolling to a finished silver copper titanium foil strip solder.

2. The method for rapidly preparing a silver-copper-titanium foil solder according to claim 1, characterized by: In the step (1), the particle size of the silver copper alloy powder is ≤100 μm and D50 is 38-53 μm; the particle size of the titanium powder or titanium hydride powder is 5-25 μm, and the sphericity of the titanium powder is ≥0.

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3. The method of quickly preparing silver-copper-titanium foil ribbon solder according to claim 1, characterized in that: The sintering in the step (1) and the intermediate annealing treatment in the step (2) are both performed under the protection of a flux.

4. The method of quickly preparing silver-copper-titanium foil ribbon solder according to claim 3, characterized by: The flux is at least one of QJ101 and QJ102.

5. The method for rapidly preparing silver-copper-titanium foil ribbon solder according to any one of claims 1 to 4, characterized in that: In the step (1), the silver copper titanium compact sintering process is: first, placing the silver copper titanium compact into a flux at 350-400 ℃ for 5-10 min, then heating at a rate of ≥8 ℃ / min to 780-800 ℃ and keeping for 5-15 min, and directly water cooling to room temperature.

6. The method for rapidly preparing silver-copper-titanium foil solder strip according to any one of claims 1 to 4, characterized in that: In the step (1), the silver copper titanium hydride compact sintering process is: first, placing the silver copper titanium hydride compact into a flux at 300-350 ℃ for 5-10 min, then heating at a rate of 4-8 ℃ / min to 650-700 ℃, and heating at a rate of ≥8 ℃ / min to 780-800 ℃ and keeping for 5-15 min, and directly water cooling to room temperature.

7. The method for rapidly preparing silver-copper-titanium foil solder according to any one of claims 1 to 4, characterized in that: In the step (2), the intermediate annealing process is: placing the solder into a flux at 650-680 ℃ for 3-10 min or heating to 720-740 ℃ under the protection of a flux by a flame, and then directly water cooling to room temperature, and the number of intermediate annealing is ≤6 times.

8. The method of quickly preparing silver-copper-titanium foil ribbon solder according to claim 1, characterized by: The vacuum annealing process in the step (3) is: vacuum degree ≤1.0×10 -3 Pa, holding for 3-10 min at 640-670 ℃, then cooling to below 250 ℃ at a rate of ≥8 ℃ / min, and the number of vacuum annealing is ≤2.

9. The method for rapidly preparing silver-copper-titanium foil ribbon solder according to any one of claims 1 to 4, characterized by: The thickness of the finished silver copper titanium foil strip solder is 0.05-0.12 mm, and the titanium content is 3-8 wt%.

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