CN115464300A - Method for processing reinforcing material for solder, composite solder and method for processing the same - Google Patents
Method for processing reinforcing material for solder, composite solder and method for processing the same Download PDFInfo
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- 238000012545 processing Methods 0.000 title claims description 13
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Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/26—Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
- B23K35/262—Sn as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/40—Making wire or rods for soldering or welding
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
- C22C30/02—Alloys containing less than 50% by weight of each constituent containing copper
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a processing method of a reinforcing material for a solder, a composite solder and a processing method thereof, wherein the raw materials of Cu powder, sn powder and Ni powder with the mass ratio of 2.5-3.0; melting raw materials containing Sn powder, bi powder and near-amorphous reinforcing material powder at 280-320 ℃, and then cooling to obtain the composite solder. The invention provides a simple, reliable and high-quality method for preparing a near-amorphous multi-phase intermetallic compound (IMC) sample, and the IMC micron particles can become a potential composite material reinforcement for improving the mechanical property of SnBi solder.
Description
Technical Field
The invention relates to the technical field of electronic packaging micro-interconnection, in particular to a processing method of a reinforcing material for a solder, a composite solder and a processing method thereof.
Background
In the field of electronic packaging and assembly, tin-based solder is an important interconnection material at chip level, packaging level and board level, and can realize the functions of electrical, signal and mechanical connection between two metal surfaces after forming a micro-welding point. The melting point of tin-based solders of common SnAgCu system, snAg system and SnCu system is 222-245 ℃, but the product yield can be ensured only by welding at low temperature because many electronic components such as Light Emitting Diodes (LEDs), flexible materials and solar panel photovoltaic solder strips are sensitive to temperature. Therefore, the SnBi solder has relatively low melting point (138 ℃), good wettability, low price and high tensile strength, and becomes an important solder in the field of low-temperature welding in the microelectronic manufacturing industry. However, snBi solder has poor ductility and exhibits a brittle fracture mode after soldering. Meanwhile, due to the brittleness of the Bi element, the SnBi solder has poor creep resistance and insufficient mechanical strength. This has hindered further development in the field of low temperature packaging.
Researches show that the method for enhancing the mechanical property of the SnBi solder alloy by adopting the micron or nano particles is an effective way for improving the mechanical property of the SnBi solder alloy. The nano Ag particle reinforced SnBi composite solder can show better mechanical property, but the shear strength is not obviously improved, and the preparation cost of the reinforcing phase is high. Intermetallic compound (IMC) Cu 6 Sn 5 The product which is common in the tin-based solder welding process can be added into SnBi solder as a reinforcing phase, and the hardness and the elastic modulus of the composite solder alloy can be effectively improved. However, reduction precipitation methods are currently used to produce Cu 6 Sn 5 The preparation process of the nano-particles is complex, and the requirements of raw materials are various. The addition of the Carbon Nanotubes (CNTs) can refine the microstructure of the Sn-Bi solder, thereby improving the strength and the mechanical property of a welding spot, but the preparation process is not easy to control, and the carbon nanotubes are easy to cause when lattice defects are formedToo short, the properties of the original carbon nanotubes are lost.
The amorphous alloy has excellent mechanical properties and is the strongest metal material (the highest yield strength and fracture toughness) so far. In recent years, although lead-free solder enhancement by intermetallic compound (IMC) particles has been studied, the effect of amorphous or near-amorphous IMCs alloy particles on SnBi solder has not been studied.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a processing method of a reinforcing material for a solder, a composite solder and a processing method thereof.
The invention is realized by the following steps:
in a first aspect, the present invention provides a method for processing a reinforcing material for solder, which comprises the steps of sintering a raw material, wherein the mass ratio of a Cu powder, a Sn powder and a Ni powder is 2.5-3.0.
In an alternative embodiment, the sintering step comprises: heating the sintering temperature from 15-25 ℃ to 450-550 ℃ within 15-25min, and preserving the heat for 20-40min; then reducing the treatment temperature to 20-25 ℃ within 100-130 min;
preferably, the vacuum degree of the sintering step is 1 × 10 -2 The following;
preferably, the sintering step applies a pressure of 45-55Mpa to the material.
In an alternative embodiment, the sintering is followed by melting and quenching solidification in sequence;
preferably, the smelting step temperature is 950-1050 ℃;
preferably, the vacuum degree of the smelting step is 1 × 10 -2 The following;
preferably, the extremely condensed solidification is the temperature of the molten mass is reduced to 20-30 ℃ within 30-60 s.
In an alternative embodiment, the melting and quench solidification is carried out in a vacuum melting melt-spun furnace;
preferably, the speed of the roller of the melt-spun furnace in the quenching solidification process is 30-40m/s.
In an optional embodiment, crushing the material obtained by quenching solidification to obtain a granular near-amorphous reinforcing material;
preferably, the pulverizing step is performed in a planetary ball mill;
preferably, the grinding ball in the crushing step is made of zirconia;
preferably, the grinding balls in the crushing step comprise large balls with the diameter of 10mm and small balls with the diameter of 5mm, and the weight ratio of the large balls to the small balls is 1.2-1.5:1;
preferably, the ball-to-feed ratio in the pulverizing step is about 18-22:1;
preferably, the crushing step adopts a wet grinding mode, the ball milling time is 60-75 hours, and the rotating speed of a ball mill is 280-320r/min;
preferably, the wet grinding is to add absolute ethyl alcohol into the ball mill tank to cover the materials and the spheres;
preferably, after wet grinding, drying the materials for 20-28h at the temperature of 50-60 ℃;
preferably, the wet milling is followed by sieving using a 2300 mesh screen to obtain particulate near amorphous reinforcement material having a size of less than 5 μm.
In an alternative embodiment, before sintering, the method further comprises pressing the mixed powder of the Cu powder, the Sn powder and the Ni powder into a bulk mixed material;
preferably, the particle diameters of the Cu powder, the Sn powder, and the Ni powder are independently 70 to 80 μm;
preferably, the mixed powder is pressed by using a graphite die, wherein the graphite die is assembled in the form of a top column, a gasket, graphite paper, a powder sample, graphite paper, a gasket and a top column;
preferably, removing impurities on the surface of the material before the smelting step;
preferably, the mixed powder is obtained by mixing the Cu powder, the Sn powder, and the Ni powder in a planetary ball mill and a stainless steel ball mill pot;
preferably, the mixing time is 8-12min, and the mixing speed is 280-320r/min.
In a second aspect, the present invention provides a composite solder containing the reinforcing material for solder obtained in any one of the above embodiments.
In an alternative embodiment, the reinforcing material for solder accounts for 0.25-1% of the total weight of the composite solder.
In a third aspect, the invention provides a processing method of composite solder, which comprises the steps of melting raw materials containing Sn powder, bi powder and near-amorphous reinforcing material powder at 280-320 ℃, and then cooling to obtain the composite solder.
In alternative embodiments, the cooling rate is from 8 to 12 ℃/min;
preferably, the composite solder is cut and then placed in molten rosin for remelting to obtain a spherical composite solder;
preferably, the weight ratio of the Sn powder to the Bi powder is 42:58;
preferably, the raw materials containing the Sn powder, the Bi powder and the near-amorphous reinforcing material powder are uniformly mixed before being melted, and pressure is maintained at 8-12Mpa for 3-5min to prepare a compact;
preferably, the raw materials containing the Sn powder, the Bi powder and the near-amorphous reinforcing material powder are mixed in a ball mill for 10-15min under the condition of 280-320r/min and uniformly mixed.
The invention has the following beneficial effects:
the near-amorphous multi-phase IMC particles prepared by the method have the advantages of low material cost and process cost, simple operation process, reliable preparation result and higher sample quality.
The invention provides a simple, reliable and high-quality method for preparing a near-amorphous multi-phase intermetallic compound (IMC) sample. Through vacuum sintering treatment, three metal elements of Cu, sn and Ni can react to generate a plurality of IMCs (Cu) 81 Sn 22 And Ni 3 Sn, etc.) products.
On the basis of obtaining the IMC sample through powder metallurgy preparation, IMC particles are uniformly mixed with Sn and Bi powder (the purity is 99.998 percent), and the mixture is smelted to prepare the composite solder alloy, and the results of various mechanical property tests show that: the IMC micron particles can become a potential composite material reinforcement for improving the mechanical property of the SnBi solder.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a flow chart of the composite solder process of the present application;
FIG. 2 is a graph of the sintering temperature of example 1 of the present application;
FIG. 3 shows the test results of the near amorphous reinforcing material obtained in example 1 in the form of particles;
(a) X-ray diffraction results of IMC, (b) differential scanning calorimetry results of IMC;
FIG. 4 is a SnBi-xIMC composite solder microstructure;
(a) SnBi-solder alloy, (b) SnBi-0.25% IMC, (c) SnBi-0.5% IMC, and (d) SnBi-1% IMC.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The present embodiment provides a method for processing a reinforcing material for solder, which comprises sintering a raw material, in which the mass ratio of Cu powder, sn powder, and Ni powder is 2.5 to 3.0.
The nanometer IMC particles are prepared by a powder metallurgy method, the quality of the obtained sample is not high, and the preparation period is overlong; the preparation of IMC particles using the reductive precipitation method requires complicated preparation of raw materials and the reaction process is susceptible to external influences. These methods can only produce single phase IMC particle samples in a single pass, and although IMC particles can effectively reduce the phase spacing of the solder in the form of heterogeneous nucleation sites in the solder mass, refine the microstructure. However, due to the defects of the mechanical properties of the IMC particles obtained in the preparation processes, the improvement of the mechanical properties of the composite solder is limited. The invention provides a method for preparing multiphase IMC particles in a near amorphous alloy form based on a mechanical alloying method, and the multiphase IMC particles are used for strengthening SnBi solder.
The invention provides a simple, reliable and high-quality method for preparing a near-amorphous multi-phase intermetallic compound (IMC) sample. Through vacuum sintering treatment, three metal elements of Cu, sn and Ni can react to generate a plurality of IMCs (Cu) 81 Sn 22 And Ni 3 Sn, etc.) products. The near-amorphous multi-phase IMC particles prepared by the method have the advantages of low material cost and process cost, simple operation process, reliable preparation result and higher sample quality.
Further, the sintering step comprises: heating the sintering temperature from 15-25 deg.C (room temperature) to 450-550 deg.C (such as 450 deg.C, 470 deg.C, 490 deg.C, 510 deg.C, 530 deg.C, 550 deg.C) within 15-25min (such as 15min, 18min, 21min, 24min, 25min, etc.), and maintaining for 20-40min (such as 20min, 25min, 30min, 35min, 40min, etc.); then reducing the treatment temperature to 20-25 deg.C (room temperature) within 100-130min (such as 100min, 110min, 120min, 130min, etc.);
preferably, the vacuum degree of the sintering step is 1 × 10 -2 The influence of air is reduced;
preferably, the sintering step applies a pressure of 45-55Mpa to the material.
Further, smelting and quenching solidification are sequentially carried out after the sintering;
preferably, the smelting step temperature is 950-1050 ℃;
preferably, the vacuum degree of the smelting step is 1 × 10 -2 The following;
preferably, the extremely condensed solidification is the temperature of the molten mass is reduced to 20-30 ℃ within 30-60 s.
The sintered sample is subjected to vacuum melting melt-spinning treatment, so that the defects of more cavities and uneven IMC distribution of the sintered sample are overcome, the melted sample is rapidly solidified, atoms are not in time to be orderly arranged and crystallized, the obtained solid alloy is of a long-range disordered structure, and crystal grains and crystal boundaries of crystalline alloy do not exist, so that a large amount of amorphous phases containing Sn and having excellent mechanical properties exist in IMC particles, and a compact, uniform and near-amorphous multi-phase intermetallic compound sample with excellent mechanical properties is obtained.
Compared with the traditional SnBi solder alloy, the near-amorphous multi-phase intermetallic compound enhanced composite solder prepared by the invention has obvious microstructure refinement and no microscopic defects.
Further, the smelting and the quenching solidification are carried out in a vacuum smelting melt-spinning furnace;
preferably, the speed of the roller of the belt-throwing furnace is 30-40m/s in the quenching solidification process, and the cooling time is adjusted by adjusting the speed of the roller.
Further, crushing the material obtained by quenching solidification to obtain a granular near-amorphous reinforcing material;
preferably, the pulverizing step is performed in a planetary ball mill;
preferably, the grinding ball in the crushing step is made of zirconia;
preferably, the grinding balls in the crushing step comprise large balls with the diameter of 10mm and small balls with the diameter of 5mm, and the weight ratio of the large balls to the small balls is 1.2-1.5:1;
preferably, the ball-to-feed ratio in the pulverizing step is about 18-22:1;
preferably, the crushing step adopts a wet grinding mode, the ball milling time is 60-75 hours, and the rotating speed of a ball mill is 280-320r/min;
preferably, the wet grinding is to add absolute ethyl alcohol into the ball mill tank to cover the materials and the spheres;
preferably, after wet grinding, drying the materials for 20-28h at the temperature of 50-60 ℃;
preferably, the wet milling is followed by sieving using a 2300 mesh screen to obtain particulate near amorphous reinforcement material having a size of less than 5 μm.
And (3) grinding the banded near-amorphous alloy by using a high-energy ball mill, sieving and drying to obtain near-amorphous multiphase IMC particles.
And grinding the reinforced material by adopting a planetary ball mill to obtain micron-sized near-amorphous multi-phase IMC particles, and sieving the material with larger particle size and then grinding the material again until the particle size meets the requirement.
Further, before sintering, pressing the mixed powder of the Cu powder, the Sn powder and the Ni powder into a massive mixed material;
preferably, the particle diameters of the Cu powder, the Sn powder, and the Ni powder are independently 70 to 80 μm;
preferably, the mixed powder is pressed by using a graphite die, wherein the graphite die is assembled in the form of a top column, a gasket, graphite paper, a powder sample, graphite paper, a gasket and a top column;
preferably, removing impurities on the surface of the material before the smelting step;
preferably, the mixed powder is obtained by mixing the Cu powder, the Sn powder, and the Ni powder in a planetary ball mill and a stainless steel ball mill pot;
preferably, the mixing time is 8-12min, and the mixing speed is 280-320r/min.
Mixing metal powder evenly and putting the mixture into a graphite mould with a cylindrical cavity, performing SPS discharge plasma sintering on a sample according to a proper temperature curve, grinding off a graphite layer on the surface of the sample after cooling, and cutting the sample into a proper size for sintering.
Ball milling is adopted and the particle size of the raw materials is limited, which is beneficial to the uniform mixing of the raw materials.
Another example of the present application can provide a composite solder containing the reinforcing material for solder obtained in any one of the above embodiments.
Further, the reinforcing material for the solder accounts for 0.25 to 1 percent of the total weight of the composite solder.
The near-amorphous multi-phase IMC particles prepared by the method can obviously enhance the shearing performance and the creep resistance of the composite solder. The modulus of elasticity of the composite solder can also be enhanced for certain specific levels of IMC (e.g., when 0.5wt% IMC is added).
The existence of the near-amorphous multi-phase IMC particles prepared by the method can promote the diffusion effect between the SnBi solder and the matrix, thereby improving the combination tightness of the joint.
The near-amorphous multi-phase intermetallic compound enhanced composite solder prepared by the invention overcomes the defect of poor ductility of the traditional SnBi solder. The addition of IMC changes the shear fracture mode of the SnBi solder, and the brittle fracture mode is changed into a mixed fracture mode with both brittleness and toughness, so that the plastic deformation capacity of the composite solder is greatly enhanced.
The other embodiment of the application can also provide a processing method of the composite solder, which is to melt raw materials containing Sn powder, bi powder and near-amorphous reinforcing material powder at 280-320 ℃ and then cool the raw materials to obtain the composite solder.
On the basis of preparing the IMC sample by powder metallurgy, IMC particles are uniformly mixed with Sn and Bi powder (the purity is 99.998 percent), and the mixture is prepared into the composite solder alloy by smelting, and the results of various mechanical property tests show that: the IMC micron particles can become a potential composite material reinforcement for improving the mechanical property of the SnBi solder.
Further, the cooling rate is 8-12 ℃/min;
preferably, the composite solder is cut and then placed in molten rosin for remelting to obtain a spherical composite solder;
preferably, the weight ratio of the Sn powder to the Bi powder is 42:58;
preferably, the raw materials containing the Sn powder, the Bi powder and the near-amorphous state reinforcing material powder are uniformly mixed before being melted, and pressure is maintained at 8-12Mpa for 3-5min to prepare a pressed block;
preferably, the raw materials containing the Sn powder, the Bi powder and the near-amorphous reinforcing material powder are mixed in a ball mill for 10-15min under the condition of 280-320r/min and uniformly mixed.
Ball milling is adopted to increase the uniformity of raw material mixing.
The features and properties of the present invention are described in further detail below with reference to examples.
Examples 1 to 3
The embodiment provides a processing method of a reinforcing material for solder, as shown in fig. 1, the specific implementation steps are as follows:
1. cu, sn and Ni powders with the particle size of 75 microns are prepared and mixed in a planetary ball mill for 10min according to the mass ratio shown in the table 1, and the rotating speed is 300r/min. The process requires placing the powder in a stainless steel ball mill jar without adding grinding balls.
TABLE 1 Metal powder quality
| Cu/g | Sn/g | Ni/g | |
| Example 1 | 14.29 | 29.65 | 4.4 |
| Example 2 | 10.58 | 27.7 | 3.91 |
| Example 3 | 12.47 | 27.56 | 4.19 |
2. And (3) assembling by using a graphite die in the form of a top column, a gasket, graphite paper, a powder sample, graphite paper, a gasket and a top column.
And (3) SPS spark plasma sintering. At a vacuum degree of 1X 10 -2 In the following vacuum environment, the furnace temperature is set to be 20-500 ℃ for 20min, then the temperature is kept at 500 ℃ for 30min, and finally the furnace is cooled for two hours. A pressure of 50MPa is always applied during this process. After the temperature curve is finished, the PLC value is regulated to 0 in a staged manner, and the sample can be taken out to finish sintering. The sintering curve is shown in fig. 2.
4. The graphite layer adhered to the surface of the cylindrical sample was polished off using 400-mesh sandpaper to obtain a contamination-free sample, and then the sample was orthogonally cut into a suitable size (capable of being loaded into a quartz test tube) by a wire cutting process.
5. And (4) vacuum melting the strip. At a vacuum degree of 1X 10 -2 In the following vacuum environment, setting electric arc heating from room temperature to 1000 ℃, then carrying out melt spinning at the roller speed of 35m/s, so that the melted sample is rapidly solidified, atoms are not in time of ordered arrangement and crystallization, and the obtained solid alloy is in a long-range disordered structure and does not have crystal grains and crystal boundaries of crystalline alloy. Obtaining the ribbon-shaped near-amorphous alloy.
6. High-energy ball milling is carried out on the strip-shaped near-amorphous alloy in a planetary ball mill. The material quality is about 3.5g, and the ball-milling effect is strengthened to the spheroid that the ball-milling ball is zirconia material and uses two kinds of sizes (big ball diameter 10mm, pellet diameter 5 mm). The ball-to-feed ratio is about 20:1, the proportion of the spheres and the materials can bring about the best ball milling effect. The rotation speed of the ball mill is 300r/min, IMC particles with the size less than 5 mu m are obtained by using a 2300-mesh screen after wet grinding (covering materials and spheres with a proper amount of absolute ethyl alcohol) for 72 hours, and then the IMC particles are dried in a vacuum drying oven at the constant temperature of 55 ℃ for 24 hours to obtain the final IMC particle additive. Characterization of phase composition of IMC particle samples by X-ray diffractionAs a result, the heat change and the mass change of the IMC particle sample obtained in example 1 were examined using a differential scanning calorimeter, and the results obtained are shown in FIG. 3, in which Cu 81 Sn 22 And Ni 3 Sn is two phases existing in the IMC particles, and simultaneously, the results of a differential scanning calorimeter show that a great amount of Sn-containing amorphous phases such as (Cu, ni) exist in the IMC particles 6 Sn 5 And (Ni, cu) 3 Sn 4 。
Examples 4 to 5:
the only difference from example 1 is: the sintering step mainly has the action temperatures of 450 ℃ and 550 ℃, and the IMC particles also contain Cu 81 Sn 22 、Ni 3 Sn、(Cu,Ni) 6 Sn 5 And (Ni, cu) 3 Sn 4 。
Comparative example 1
The only difference from example 1 is: the sintering step mainly has the action temperature of 800 ℃, and the IMC particles also contain Cu 81 Sn 22 、Ni 3 Sn、(Cu,Ni) 6 Sn 5 And (Ni, cu) 3 Sn 4 However, the phase composition ratio of the particles is greatly different from that of the particles in example 1, so that the effect of improving the performance of the solder applied to the solder is not obvious in the examples.
Comparative example 2
The only difference from example 1 is: the speed of the roller is 15m/s, so that the temperature of the molten material is reduced to 20-30 ℃ (room temperature can be understood to be more than 1 min), and the IMC particles also contain Cu 81 Sn 22 、Ni 3 Sn、(Cu,Ni) 6 Sn 5 And (Ni, cu) 3 Sn 4 Because the cooling speed is relatively slow, crystal grain boundaries of crystalline alloys can be generated, and the effect of improving the performance of the solder is not as good as that of amorphous IMC particles.
TABLE 2 Effect of IMC particles from different examples on the Properties of composite solders
Examples 6 to 9
The embodiment provides a composite solder, and the specific processing method comprises the following steps:
1. 0wt%, 0.25wt%, 0.5wt% and 1wt% of the IMC particles obtained in example 1 were mixed with Sn and Bi powders (each having a purity of 99.998% and a mass ratio of the Sn to Bi powders of 42) respectively for 10min using a ball mill at a rotation speed of 300r/min. Then, the four groups of powders were each pressed into a lump sample using a tablet press (pressure 10MPa, holding pressure for 3 minutes).
2. And (3) melting the blocky samples with different IMC contents in the rosin covering agent for 10min at the temperature of 300 ℃ by using a flat plate heating furnace, and cooling at the speed of 10 ℃/min to obtain the IMC particle enhanced SnBi composite solder. In order to test the mechanical property of the composite solder conveniently, the composite solder is cut into small metal blocks according to the quality, and the small metal blocks are subjected to remelting treatment in molten rosin, washed by absolute ethyl alcohol after cooling and dried to prepare the high-quality IMC particle enhanced SnBi composite solder ball.
Comparative example 3
The only difference from example 6 is: in the composite solder, the content of IMC particles is 3wt%.
And (3) performance testing:
to evaluate the effect of this near-amorphous multiphase IMC on SnBi solder microstructure and mechanical properties, composite solder micro-solder joints were prepared by reflow soldering composite solder balls (500 μm diameter) on custom PCB board copper pads (320 μm diameter) using a BGA rework station. The obtained microwelded sample was cold-set, ground and polished, and the microstructure of the microwelded spot was observed by a scanning electron microscope, as shown in fig. 4. The microstructure of the alloy was significantly refined after addition of IMC compared to SnBi alloy, with the refinement of the IMC particles by 0.5wt% being most significant. The shear properties and creep resistance of the composite solder were then specifically evaluated by ball-pushing shear test and nanoindentation test, and the results are shown in table 2.
TABLE 3 Performance of SnBi-xIMC composite solders
This example is based on a mechanical alloying method to prepare multiphase IMC particles in the form of a near amorphous alloy and use them for SnBi solder reinforcement. Smelting and quenching solidification equipment are used to obtain an IMC sample in a near-amorphous alloy form, so that the IMC which can be tightly combined with a soldering flux has more excellent mechanical properties. The micron-sized particle reinforcement is successfully obtained by a high-energy ball milling method, and the phase composition of the IMC particles is characterized by X-ray diffraction. Finally, the micron-sized particle reinforcement is uniformly mixed with SnBi solder powder and is pressed and formed, a high-quality composite solder sample is efficiently and conveniently prepared by using an alloy smelting method, and the problems of cost control, preparation process controllability and the like are optimized to a certain extent while the strength and the mechanical property of the SnBi solder are effectively improved.
1. The near-amorphous multi-phase IMC particles prepared in the embodiment have the advantages of low material cost and process cost, simple operation process, reliable preparation result and high sample quality.
2. Compared with the traditional SnBi solder alloy, the near-amorphous multi-phase intermetallic compound enhanced composite solder prepared in the embodiment has the advantages of obvious microstructure refinement and no microscopic defects.
3. The near-amorphous multi-phase IMC particles prepared in the embodiment can obviously enhance the shearing performance and the creep resistance of the composite solder. The modulus of elasticity of the composite solder can also be enhanced for certain specific levels of IMC (e.g., when 0.5wt% IMC is added).
4. The existence of the near-amorphous multi-phase IMC particles prepared in the embodiment can promote the diffusion effect between the SnBi solder and the matrix, thereby improving the bonding tightness of the joint.
5. The near-amorphous multi-phase intermetallic compound enhanced composite solder prepared in the embodiment overcomes the defect of poor ductility of the traditional SnBi solder. The addition of IMC changes the shear fracture mode of the SnBi solder, and the brittle fracture mode is changed into a mixed fracture mode with both brittleness and toughness, so that the plastic deformation capacity of the composite solder is greatly enhanced.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A processing method of a reinforcing material for a solder is characterized in that raw materials of Cu powder, sn powder and Ni powder with the mass ratio of 2.5-3.0.
2. The method for processing a reinforcing material for solder according to claim 1, wherein the sintering step comprises: heating the sintering temperature from 15-25 ℃ to 450-550 ℃ within 15-25min, and preserving the heat for 20-40min; then reducing the treatment temperature to 20-25 ℃ within 100-130 min;
preferably, the vacuum degree of the sintering step is 1 × 10 -2 The following;
preferably, the sintering step applies a pressure of 45-55Mpa to the material.
3. The method for processing the reinforcing material for solder according to claim 1, wherein the sintering is followed by melting and quenching solidification in this order;
preferably, the smelting step temperature is 950-1050 ℃;
preferably, the vacuum degree of the smelting step is 1 × 10 -2 The following;
preferably, the extremely condensed solidification is the temperature of the molten mass is reduced to 20-30 ℃ within 30-60 s.
4. The method for processing a reinforcing material for solder according to claim 3, wherein the melting and the quenching solidification are carried out in a vacuum melting and melting furnace;
preferably, the speed of the roller of the melt-spun furnace in the quenching solidification process is 30-40m/s.
5. The method for processing the reinforcing material for solder according to claim 3 or 4, wherein the material obtained by the rapid cooling solidification is pulverized to obtain a granular near-amorphous reinforcing material;
preferably, the pulverizing step is performed in a planetary ball mill;
preferably, the grinding ball in the crushing step is made of zirconia;
preferably, the grinding balls in the crushing step comprise large balls with the diameter of 10mm and small balls with the diameter of 5mm, and the weight ratio of the large balls to the small balls is 1.2-1.5:1;
preferably, the ball-to-feed ratio in the pulverizing step is about 18-22:1;
preferably, the crushing step adopts a wet grinding mode, the ball milling time is 60-75 hours, the rotating speed of a ball mill is 280-320r/min,
preferably, the wet grinding is to add absolute ethyl alcohol into the ball mill tank to cover the materials and the spheres;
preferably, after wet grinding, drying the material for 20-28h at the temperature of 50-60 ℃;
preferably, the wet milling is followed by sieving using a 2300 mesh screen to obtain particulate near amorphous reinforcement material having a size of less than 5 μm.
6. The method of processing a reinforcing material for solder according to claim 1, further comprising pressing a mixed powder of the Cu powder, the Sn powder, and the Ni powder into a lump-like mixed material before sintering;
preferably, the particle diameters of the Cu powder, the Sn powder, and the Ni powder are independently 70 to 80 μm;
preferably, the mixed powder is pressed by using a graphite die, wherein the graphite die is assembled in the form of a top column, a gasket, graphite paper, a powder sample, graphite paper, a gasket and a top column;
preferably, impurities on the surface of the material are removed before the smelting step;
preferably, the mixed powder is obtained by mixing the Cu powder, the Sn powder, and the Ni powder in a planetary ball mill and a stainless steel ball mill pot;
preferably, the mixing time is 8-12min, and the mixing speed is 280-320r/min.
7. A composite solder, characterized by containing the reinforcing material for solder obtained in any one of claims 1 to 6.
8. The composite solder according to claim 7, characterized in that the reinforcing material for solder accounts for 0.25-1% of the total weight of the composite solder.
9. A method for processing the composite solder according to claim 7 or 8, characterized in that the raw materials containing Sn powder, bi powder and near-amorphous reinforcing material powder are melted at 280-320 ℃ and then cooled to obtain the composite solder.
10. The method for processing a reinforcing material for solder according to claim 9, wherein the cooling rate is 8 to 12 ℃/min;
preferably, the composite solder is cut and then placed in molten rosin for remelting to obtain a spherical composite solder;
preferably, the weight ratio of the Sn powder to the Bi powder is 42:58;
preferably, the raw materials containing the Sn powder, the Bi powder and the near-amorphous state reinforcing material powder are uniformly mixed before being melted, and pressure is maintained at 8-12Mpa for 3-5min to prepare a pressed block;
preferably, the raw materials containing the Sn powder, the Bi powder and the near-amorphous reinforcing material powder are mixed in a ball mill for 10-15min under the condition of 280-320r/min and uniformly mixed.
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| KR20030034688A (en) * | 2001-10-26 | 2003-05-09 | 한국과학기술원 | Composite solders and process method of composite solders |
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| JP2019209361A (en) * | 2018-06-05 | 2019-12-12 | 株式会社日本スペリア社 | Lead-free solder joint material and joint part thereof |
| CN110773901A (en) * | 2019-09-29 | 2020-02-11 | 昆明理工大学 | Preparation method of SnBi lead-free composite solder |
| CN114799616A (en) * | 2022-04-28 | 2022-07-29 | 桂林电子科技大学 | High-entropy intermetallic compound material, preparation method thereof and electronic solder |
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| KR20030034688A (en) * | 2001-10-26 | 2003-05-09 | 한국과학기술원 | Composite solders and process method of composite solders |
| CN108251670A (en) * | 2016-12-28 | 2018-07-06 | 北京有色金属研究总院 | The preparation method of compound alloy between refractory metal |
| CN107999994A (en) * | 2017-11-22 | 2018-05-08 | 深圳市福英达工业技术有限公司 | Micrometer/nanometer granule enhancement type composite solder and preparation method thereof |
| JP2019209361A (en) * | 2018-06-05 | 2019-12-12 | 株式会社日本スペリア社 | Lead-free solder joint material and joint part thereof |
| CN110773901A (en) * | 2019-09-29 | 2020-02-11 | 昆明理工大学 | Preparation method of SnBi lead-free composite solder |
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