CN113102914B - High-strength anti-aging composite solder sheet and preparation method thereof - Google Patents
High-strength anti-aging composite solder sheet and preparation method thereof Download PDFInfo
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- CN113102914B CN113102914B CN202110407604.8A CN202110407604A CN113102914B CN 113102914 B CN113102914 B CN 113102914B CN 202110407604 A CN202110407604 A CN 202110407604A CN 113102914 B CN113102914 B CN 113102914B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
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- 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
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Abstract
The invention discloses a high-strength anti-aging composite solder sheet and a preparation method thereof, relating to the technical field of solder sheets, and the high-strength anti-aging composite solder sheet comprises: the composite welding flux comprises two welding flux sheets, two copper-nickel nanowire coating layers are arranged between the two welding flux sheets, and a composite welding flux slurry layer is arranged between the two copper-nickel nanowire coating layers. Compared with the prior art, the invention has the beneficial effects that: aiming at the limitation of the prior art, the invention obviously improves the consistency of the quality and the performance of the solder sheet while reducing the material cost, and improves the strength and the thermal aging resistance of the solder sheet while not influencing the solderability and the service interface reliability of the solder sheet.
Description
Technical Field
The invention relates to the technical field of solder sheets, in particular to a high-strength anti-aging composite solder sheet and a preparation method thereof.
Background
The power modules such as the IGBT and the like are widely applied to the fields of smart power grids, electric automobiles and the like. Typical power module packaging structures typically include two to three solder layers with different melting points to achieve mechanical, thermal and electrical interconnection between the semiconductor chip, the terminals, the insulating substrate and the metal base plate. At present, with the continuous improvement of the integration degree of a power module, the thickness of each solder connection layer in a packaging structure is also continuously reduced, and because the thermal resistivity of different materials in the packaging structure has great difference, the joule heat generated in the service process of the module is usually concentrated on one side of a chip and is larger than that on one side of a substrate, and the phenomenon inevitably causes great temperature gradient inside the solder interconnection layer, and the aging and failure of the packaging interconnection structure are accelerated under the combined action of external complex working conditions. Therefore, there is an urgent need to develop a high-performance lead-free solder, which greatly improves the strength and aging resistance of the solder layer of the power electronic module package, thereby improving the package reliability of the power module.
In the prior art, a solder interconnection layer with higher strength and relatively good thermal aging resistance is obtained by means of nano silver paste sintering, composite silver paste sintering, adding reinforcing phase particles to a traditional solder (such as patent CN201810361358.5, patent CN201810383172.x, patent CN201910384352.4, patent CN201610948850.3 and the like), but the method has high material cost and poor product quality consistency. In other methods (for example, patent No. cn201710149734.x) for preparing a composite solder sheet by soaking zinc-based or tin-based solder with foamed metal and rolling, a "support skeleton" with high strength is formed inside the solder sheet to improve the mechanical strength of the solder sheet itself, but the foamed metal material is still dispersed on the surface of the solder sheet, which inevitably affects the later weldability of the formed solder sheet and the interface reliability in the service process.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a high-strength anti-aging solder sheet and a preparation method thereof.
In order to achieve the purpose, the invention is realized by the following technical scheme: a high-strength aging-resistant composite solder sheet, comprising: two layers of nanowire coating layers are arranged between the two solder sheets, and a composite solder paste layer is arranged between the two layers of nanowire coating layers;
The nanowire coating layer is prepared from nanowire suspension through applying ultrasonic vibration in X and Y directions and drying for 20-30 minutes at 40 ℃ in vacuum, and the thickness of the nanowire coating layer is 5-20 micrometers.
The preparation process of the nanowire turbid liquid comprises the following steps:
0.2g of nanowire with the diameter of 100-200 nm and the length of 10-20 nm is weighed and placed in 8ml of ethanol solution, 0.025g of polyvinylpyrrolidone and 0.01g of oleic acid are added, and ultrasonic dispersion is carried out for 15 minutes.
The composite solder paste layer is prepared by applying ultrasonic vibration in X and Y directions to composite solder paste for 10 minutes, then applying ultrasonic vibration in Z direction for 15 minutes, and then drying for 20-40 minutes at 40 ℃ in vacuum, wherein the total thickness of the composite solder paste layer and the single-layer nanowire coating layer is 50-100 microns.
The composite solder paste is prepared from double-plating layer nano powder and solder powder.
The preparation process of the double-coating nano powder comprises the following steps:
(1) weighing a certain mass of nano powder which is subjected to decontamination and dispersion treatment and has an average particle size of 150 nanometers, adding the nano powder into 0.2mol/L sodium hydroxide solution, and performing electromagnetic stirring for 5-10 minutes to perform coarsening pretreatment;
(2) performing multi-pass centrifugal filtration on the nano powder, and adding the coarsened nano powder obtained by washing with deionized water into the solution containing 8.5-10.5g/L SnCl 2Performing sensitization treatment by applying electromagnetic stirring in the ethanol solution, wherein the ratio of the nano powder is 0.5-0.8g/L, the activation temperature is 40-60 ℃, and the sensitized nano powder is subjected to multi-pass centrifugal filtration;
(3) washing the nano powder with deionized water, adding the washed nano powder into a solution containing 0.04-0.08mol/L silver nitrate and 8.25-10.55mol/L ammonia water, performing electromagnetic stirring for 15 minutes for activation treatment, then adding 0.42-0.86mol/L formaldehyde and 0.55-0.65mol/L ethanol, and the balance being deionized water, uniformly stirring for 10-15 minutes, and adding the silver ammonia solution into the solution at the temperature of 10-15 ℃: 0.15-0.24mol/L silver nitrate solution and 11.25-14.45mol/L ammonia water, adjusting the pH value to 10-12, performing powder silvering, performing electromagnetic stirring for 2-3 hours, performing multi-pass centrifugal filtration and vacuum low-temperature drying to obtain silvered nano powder;
(4) adding silver-plated nano powder to 0.5g/LPdCl2Performing secondary activation treatment in the solution, wherein electromagnetic stirring is applied in the activation process, the activation temperature is 40-60 ℃, and the activation time is 15-30 minutes;
(5) and adding 0.3-0.6g/L silver-plated nano powder subjected to secondary activation into a nickel plating solution for nickel plating, electromagnetically stirring for 5-10 minutes in the nickel plating process, wherein the nickel plating temperature is 50-80 ℃, and after the nickel plating is finished, performing multi-pass centrifugal filtration and vacuum low-temperature drying to obtain the double-plating-layer nano powder.
The formula of the nickel plating solution is as follows:
18-22g/L NiSO4·7H2o, 25-32g/L N2H 4. H2O, 8-12g/L sodium tartrate, 18.2-25.6g/L sodium citrate, 24-36g/L (NH)4)2SO4，4.5％-6％NH3·H2O, 3.5-6.5g/L polyvinylpyrrolidone and 1.2-2.2g/L sodium vinylsulfonate.
The preparation process of the composite solder paste is as follows:
weighing a certain mass of double-plating layer nano powder and a certain mass of welding powder, wherein the mass fraction of the double-plating layer nano powder is 0.05-0.15%, the balance is the welding powder, adding a proper amount of water-soluble no-clean soldering flux into the double-plating layer nano powder and the welding powder to ensure that the volume ratio of the soldering flux to solid powder (including the welding powder and the double-plating layer nano powder) is 3:1-5:1, and fully and mechanically stirring the mixed liquid to uniformly mix the mixed liquid to prepare the composite solder paste.
A preparation method of a high-strength anti-aging composite solder sheet comprises the following steps:
(1) taking two solder sheets, and pretreating the solder sheets;
(2) placing the treated solder sheet on an ultrasonic vibration operation table, uniformly coating a layer of cleaning-free soldering flux on the surface of the solder sheet, sequentially preparing a nanowire coating layer, a composite solder paste layer and a nanowire coating layer on the surface of the solder sheet, uniformly coating the cleaning-free soldering flux on the surface of another solder sheet, and covering the surface coated with the soldering flux downwards on the surface of a multilayer coating to obtain a sandwich structure with the total thickness of 250-350 micrometers;
(3) Placing the sandwich structure in a soldering terminal forming die pre-designed in a hot press, preheating the hot press to 200 ℃, and performing hot pressing at the pressure of 6-12Mpa and maintaining the pressure at 200-220 ℃ for 2-5 minutes, wherein the sandwich structure is pressed to 150-200 microns;
(4) taking out the composite solder sheet, cooling the composite solder sheet to 80-100 ℃, performing hot rolling, and further rolling the composite solder sheet into a 100-150 micron solder sheet; and taking out the rolled composite solder sheet, and removing dirt and oxides on the surface.
The pretreatment steps of the solder sheet are as follows:
preparing two solder sheets with the thickness of 100 microns and smooth surfaces, cleaning the surfaces of the solder sheets with acetone, cleaning the surfaces of the solder sheets with ethanol for the second time, and drying the solder sheets after cleaning.
Compared with the prior art, the invention has the beneficial effects that:
the composite structure solder sheet which is adjustable in thickness, controllable in components and suitable for being used in a service environment with a large temperature gradient is prepared on the basis of a copper-nickel nanowire wet laying process, a titanium nitride reinforced phase double-plating layer modification process, a nanowire and reinforced phase double-layer wet laying process and a semi-solid hot-pressing rolling process.
Aiming at the limitation of the prior art, the invention obviously improves the consistency of the quality and the performance of the solder sheet while reducing the material cost, and improves the strength and the thermal aging resistance of the solder sheet while not influencing the solderability and the service interface reliability of the solder sheet.
Drawings
FIG. 1 is a schematic structural diagram of a copper-nickel nanowire coating layer laid on a solder sheet;
FIG. 2 is a schematic view of a solder sheet on which a composite solder paste layer is laid;
FIG. 3 is a schematic structural diagram of a copper-nickel nanowire coating layer laid on a solder sheet;
FIG. 4 is a schematic view of the overall structure of the composite solder sheet;
FIG. 5 is example 2 test data;
FIG. 6 is example 3 test data;
FIG. 7 is example 3 test data;
FIG. 8 is example 3 test data;
FIG. 9 is example 3 test data;
FIG. 10 shows the results of the test of example 4.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the present application.
Example 1:
preparing a nanowire turbid liquid:
weighing 0.2g of copper-nickel nanowires with the diameter of 100 nanometers and the length of 10-nanometers, putting the copper-nickel nanowires into 8ml of ethanol solution, adding 0.025g of polyvinylpyrrolidone and 0.01g of oleic acid, and carrying out ultrasonic dispersion for 15 minutes.
The copper-nickel nanowires may be replaced by iron-based alloy nanowires, other copper-based alloy nanowires, nickel-based alloy nanowires, and the like.
Preparing double-plating titanium nitride nano powder:
weighing titanium nitride nanopowder which is subjected to decontamination and dispersion treatment and has the average particle size of 150 nanometers in a certain mass, wherein the titanium nitride nanopowder can be replaced by nanoscale powder with high melting point and good heat conductivity such as aluminum oxide, silicon carbide, titanium carbide, diamond and the like, in the embodiment, the titanium nitride nanopowder is added into 0.2mol/L sodium hydroxide solution, electromagnetic stirring is carried out for 5 minutes, roughening pretreatment is carried out, multi-pass centrifugal filtration is carried out, and roughened titanium nitride nanopowder obtained by washing with deionized water is added into the solution containing 8.5g/L SnCl2Performing sensitization treatment by applying electromagnetic stirring in the ethanol solution, wherein the ratio of titanium nitride nano powder is 0.5g/L, the activation temperature is 40 ℃, the sensitized titanium nitride nano powder is subjected to multi-pass centrifugal filtration, deionized water is added into the solution containing 0.04mol/L silver nitrate and 8.25mol/L ammonia water after being cleaned, electromagnetic stirring is applied for activation treatment for 15 minutes, then 0.42mol/L formaldehyde and 0.55mol/L ethanol are added, and the balance is deionized water, and uniform stirring is performed for 10 minutes; to this solution was added a silver ammonia solution at 10 degrees celsius: 0.15mol/L silver nitrate solution and 11.25mol/L ammonia water, adjusting the pH value to 10, carrying out silver plating on the titanium nitride powder, applying electromagnetic stirring for 2 hours, and after the silver plating is finished, carrying out multi-pass centrifugal filtration and vacuum low-temperature drying to obtain silver-plated titanium nitride nano powder; adding silver-plated titanium nitride nanopowder to 0.5g/LPdC l2Performing secondary activation treatment in the solution, wherein electromagnetic stirring is applied in the activation process, the activation temperature is 40 ℃, and the activation time is 15 minutes; adding the silver-plated titanium nitride nano powder of 0.3g/L after secondary activation into nickel plating solution for nickel plating, and applying the silver-plated titanium nitride nano powder in the nickel plating processElectromagnetic stirring, nickel plating time is 5 minutes, the nickel plating temperature is 50 ℃, and after nickel plating is finished, double-plating titanium nitride nano powder is obtained through multi-pass centrifugal filtration and vacuum low-temperature drying.
The diffusion speed of nickel in the tin-based solder is far higher than that of silver, but the nickel is easy to form firm metallurgical bonding with the tin-based solder, and the nickel coating on the outermost layer can form a stable bonding interface with the solder through diffusion in the subsequent hot rolling and welding processes. Meanwhile, the silver plating layer of the inner layer is relatively stable, the titanium nitride powder can be wrapped and fixed in the solder for a long time, the stabilizing and supporting effects are achieved, and the contribution is made to the improvement of the strength and the ageing resistance of the solder sheet.
The formula of the nickel plating solution is as follows:
18g/L NiSO4·7H2O，25g/L N2H4·H2o, 8g/L sodium tartrate, 18.2g/L sodium citrate, 4g/L (NH)4)2SO，g/LNH3·H2O, 3.5g/L polyvinylpyrrolidone and 1.2g/L sodium vinylsulfonate.
Preparing composite solder paste:
weighing a certain mass of double-coating titanium nitride nanopowder and a certain mass of welding powder with the average diameter of 30 microns, wherein the mass fraction of the double-coating titanium nitride nanopowder is 0.05%, and the balance is welding powder, adding a proper amount of water-soluble no-clean soldering flux into the double-coating titanium nitride nanopowder and the welding powder to ensure that the volume ratio of the soldering flux to solid powder (including the welding powder and the double-coating titanium nitride nanopowder) is 3:1-5:1, and fully and mechanically stirring the mixed liquid to uniformly mix the two powders to prepare the composite soldering flux paste.
The solder powder is tin-based solder powder, the melting point of the solder powder should be slightly higher than that of the solder sheet, and the solder powder is used in this embodiment
Processing the solder sheet:
preparing two solder sheets with 100 μm thickness and smooth and flat surface, determining the solder sheet area according to the amount of the suspension of nanowires, wherein the area of each solder sheet is not more than 10cm2Cleaning the surface of the solder sheet with acetone, cleaning with ethanol for the second time, and blowing after cleaningAnd (5) drying.
The solder sheet may be a tin-silver-copper alloy solder sheet, a tin-silver alloy solder sheet, a tin-copper alloy solder sheet, a tin-bismuth alloy solder sheet, an indium-tin alloy solder sheet, or the like.
Manufacturing a high-strength anti-aging composite solder sheet:
under a clean operation environment, the processed tin-silver-copper solder sheet is placed on an ultrasonic vibration operation table, a layer of no-clean soldering flux is uniformly coated on the surface of the tin-silver-copper substrate solder sheet, about 4ml of copper-nickel nanowire suspension liquid is absorbed by a thick dropper and coated on the surface of the tin-silver-copper substrate solder sheet, ultrasonic vibration in the X direction and the Y direction is simultaneously applied to uniformly spread the tin-silver-copper substrate solder sheet, after the suspension is uniformly spread over the surface of the processed solder sheet, the tin-silver-copper substrate solder sheet is dried for 20 minutes at 40 ℃ in vacuum for later use, and at the moment, the thickness of the copper-nickel nanowire coating on the surface of the solder sheet is 5 microns as shown in figure 1. Subsequently, the prepared composite solder paste is dripped on the surface layer of the copper-nickel nanowire coating on the surface of the soldering lug by adopting a similar operation method, ultrasonic vibration in X and Y directions is simultaneously applied for 10 minutes, ultrasonic vibration in Z direction is further applied for 15 minutes, then vacuum drying at 40 ℃ is carried out, and after the drying, the total thickness of the two layers of coatings on the surface of the soldering lug is 50 micrometers, as shown in figure 2. Then, sucking about 4ml of copper-nickel nanowire suspension liquid drop by using a wide-mouthed dropper again to coat the existing coating surface on the surface of the soldering lug, simultaneously applying ultrasonic vibration in the X direction and the Y direction to uniformly spread the copper-nickel nanowire suspension liquid, and after the suspension liquid is uniformly paved on the surface, drying the copper-nickel nanowire suspension liquid for 20 minutes at vacuum 40 ℃, wherein the total thickness of the three-layer coating on the surface of the soldering lug is 55 micrometers, as shown in fig. 3. And taking out another solder sheet which is cleaned initially, uniformly coating the surface with the no-clean soldering flux, and covering the surface coated with the soldering flux downwards on the surface of the multilayer coating to obtain a similar sandwich structure as shown in figure 4, wherein the total thickness of the sandwich structure is 250 microns.
The number of piles on nano wire coating layer and the number of piles on composite solder paste layer all can be the multilayer, and the number of piles on nano wire coating layer is 2 in this embodiment, and the number of piles on composite solder paste layer is 1.
And finally, placing the sandwich structure in a soldering terminal forming die pre-designed in a hot press, preheating the hot press to 200 ℃, starting hot pressing at 6Mpa, maintaining the pressure at 200 ℃ for 2 minutes, and pressing the sandwich structure to 150 micrometers. And then taking out the composite structure soldering lug, air cooling to 80 ℃, carrying out hot rolling, and further rolling the composite structure soldering lug into a 100-micron soldering lug. And finally, taking out the rolled solder, and removing dirt and oxides on the surface to obtain the final product of the invention.
Example 2: shear strength test of high strength aging resistant composite solder sheet
The composite solder sheet is used as interconnection solder, a 5mm multiplied by 5mm copper sheet is subjected to reflow soldering to form a Cu/solder/Cu interconnection structure, a Cu substrate can be replaced by other substrates such as Ni, Si, SiC, AlN, gallium nitride and the like, the Cu substrate is adopted in the embodiment, a DAGE shear force tester is used for testing the shear strength of the sample at normal temperature, the control group solder is SAC305 solder, and 20 parallel samples are tested in the experimental group and the control group.
And (3) testing results: the average shear strength of the Cu/solder/Cu interconnect structure prepared from the composite structure solder sheet of the present invention is significantly higher (about 22.5% improvement) than the control sample.
Example 3: constant temperature thermal aging test
The experimental group and the control group both adopt the Cu/solder/Cu interconnection structure, are placed in a vacuum constant-temperature environment at 100 ℃ and 120 ℃ for constant-temperature heat aging for 484 hours, and in the experimental process, one sample is taken out from the experimental group and the control group respectively at 0 hour, 169 hours, 324 hours and 484 hours to observe an interface intermetallic compound (Cu)6Sn5And Cu3Sn) to determine the constant temperature thermal aging resistance of the solder layer.
And (3) testing results: the growth speed of the two interface intermetallic compounds of the Cu/solder/Cu interconnection structure prepared by the invention is obviously lower than that of a control group under the aging conditions of 100 ℃ and 120 ℃.
Example 4: large temperature gradient aging test
The experimental device is a self-made temperature gradient generation device based on a constant-temperature heating piece and a semiconductor refrigerating piece, a Cu/solder/Cu interconnection structure is still adopted in a sample structure, but in order to achieve a temperature gradient not lower than 1000K/cm in a welding seam, the structural size of the sample is shown in figure 5 according to a simulation calculation result. The aging test duration of the large temperature gradient is 600 hours, and the reliability of the welding seam is judged according to the integrity degree of the hot end interconnection interface and the shape and the distribution condition of intermetallic compounds in the welding seam after the test.
And (3) testing results: the intermetallic compounds in the Cu/solder/Cu interconnection welding seam prepared by the composite solder sheet are dispersed and distributed without obvious sensible heat migration, while the control group has obvious heat migration phenomenon that the intermetallic compounds of copper and tin are gathered at one end of the welding seam.
In conclusion, the invention well promotes the mechanical properties of the composite solder sheet such as shearing and the like, enhances the thermal aging resistance of the interconnection welding seam, and enhances the service reliability of the welding seam under large temperature gradient.
The foregoing description is only exemplary of the preferred embodiments of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the features described above have similar functions to (but are not limited to) those disclosed in this application.
Claims (3)
1. A high strength, aging resistant composite solder sheet, comprising: two layers of nanowire coating layers are arranged between the two solder sheets, and a composite solder paste layer is arranged between the two layers of nanowire coating layers;
The nanowire coating layer is prepared by applying ultrasonic vibration in X and Y directions to nanowire suspension and drying for 20-30 minutes at 40 ℃ in vacuum, and the thickness of the nanowire coating layer is 5-20 micrometers;
the preparation process of the nanowire turbid liquid comprises the following steps: weighing 0.2g of nanowire with the diameter of 100-200 nanometers and the length of 10-20 nanometers, placing the nanowire in 8ml of ethanol solution, adding 0.025g of polyvinylpyrrolidone and 0.01g of oleic acid, and performing ultrasonic dispersion for 15 minutes;
the composite solder paste layer is prepared by applying ultrasonic vibration in X and Y directions for 10 minutes, then applying ultrasonic vibration in Z direction for 15 minutes, and then drying for 20-40 minutes at 40 ℃ in vacuum, wherein the total thickness of the composite solder paste layer and the single-layer nanowire coating layer is 50-100 micrometers;
the composite solder paste is prepared from double-plating layer nano powder and welding powder;
the preparation process of the double-coating nano powder is as follows:
(1) weighing a certain mass of nano powder which is subjected to decontamination and dispersion treatment and has an average particle size of 150 nanometers, adding the nano powder into 0.2mol/L sodium hydroxide solution, and performing electromagnetic stirring for 5-10 minutes to perform coarsening pretreatment;
(2) performing multi-pass centrifugal filtration on the nano powder, and adding coarsened nano powder obtained by washing with deionized water into the solution containing 8.5-10.5g/L SnCl 2Performing sensitization treatment by applying electromagnetic stirring in the ethanol solution, wherein the ratio of the nano powder is 0.5-0.8g/L, the activation temperature is 40-60 ℃, and the sensitized nano powder is subjected to multi-pass centrifugal filtration;
(3) washing the nano powder with deionized water, adding the washed nano powder into a solution containing 0.04-0.08mol/L silver nitrate and 8.25-10.55mol/L ammonia water, performing electromagnetic stirring for 15 minutes for activation treatment, then adding 0.42-0.86mol/L formaldehyde and 0.55-0.65mol/L ethanol, and the balance being deionized water, uniformly stirring for 10-15 minutes, and adding the silver ammonia solution into the solution at the temperature of 10-15 ℃: 0.15-0.24mol/L silver nitrate solution and 11.25-14.45mol/L ammonia water, adjusting the pH value to 10-12, performing powder silvering, performing electromagnetic stirring for 2-3 hours, performing multi-pass centrifugal filtration and vacuum low-temperature drying to obtain silvered nano powder;
(4) adding silver-plated nano powder to 0.5g/LPdCl2Carrying out secondary activation treatment in the solution,electromagnetic stirring is applied in the activation process, the activation temperature is 40-60 ℃, and the activation time is 15-30 minutes;
(5) adding 0.3-0.6g/L silver-plated nano powder subjected to secondary activation into a nickel plating solution for nickel plating, performing electromagnetic stirring in the nickel plating process, performing nickel plating for 5-10 minutes at the nickel plating temperature of 50-80 ℃, and performing multi-pass centrifugal filtration and vacuum low-temperature drying after the nickel plating is finished to obtain double-plating-layer nano powder;
The formula of the nickel plating solution is as follows:
18-22g/L NiSO4·7H2O，25-32g/L N2H4·H2o, 8-12g/L sodium tartrate, 18.2-25.6g/L sodium citrate, 24-36g/L (NH)4)2SO4，4.5％-6％NH3·H2O, 3.5-6.5g/L polyvinylpyrrolidone, 1.2-2.2g/L sodium vinylsulfonate;
the preparation process of the composite solder paste is as follows:
weighing a certain mass of double-plating layer nano powder and a certain mass of welding powder, wherein the mass fraction of the double-plating layer nano powder is 0.05-0.15%, and the balance is the welding powder, adding a proper amount of water-soluble no-clean soldering flux into the double-plating layer nano powder and the welding powder to ensure that the volume ratio of the soldering flux to the solid powder is 3:1-5:1, wherein the solid powder comprises the welding powder and the double-plating layer nano powder, and fully and mechanically stirring the mixed liquid to uniformly mix the mixed liquid to prepare the composite solder paste.
2. A method for producing a high-strength, aging-resistant composite solder sheet according to claim 1, characterized by comprising the steps of:
(1) taking two solder sheets, and pretreating the solder sheets;
(2) placing the treated solder sheet on an ultrasonic vibration operation table, uniformly coating a layer of cleaning-free soldering flux on the surface of the solder sheet, sequentially preparing a nanowire coating layer, a composite solder paste layer and a nanowire coating layer on the surface of the solder sheet, uniformly coating the cleaning-free soldering flux on the surface of another solder sheet, and covering the surface coated with the soldering flux downwards on the surface of a multilayer coating to obtain a sandwich structure with the total thickness of 250-350 micrometers;
(3) Placing the sandwich structure in a soldering terminal forming die pre-designed in a hot press, preheating the hot press to 200 ℃, and performing hot pressing at the pressure of 6-12Mpa and maintaining the pressure at 200-220 ℃ for 2-5 minutes, wherein the sandwich structure is pressed to 150-200 microns;
(4) taking out the composite solder sheet, cooling the composite solder sheet to 80-100 ℃, performing hot rolling, and further rolling the composite solder sheet into a 100-150 micron solder sheet; and taking out the rolled composite solder sheet, and removing dirt and oxides on the surface.
3. The method for preparing a high-strength aging-resistant composite solder sheet according to claim 2, characterized in that the solder sheet is pretreated as follows:
preparing two solder sheets with the thickness of 100 microns and smooth surfaces, cleaning the surfaces of the solder sheets with acetone, cleaning the surfaces of the solder sheets with ethanol for the second time, and drying the solder sheets after cleaning.
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