CN117718636A - Process for obtaining high-strength high-toughness nanoparticle tin-based composite solder through gradual speed-change cooling - Google Patents
Process for obtaining high-strength high-toughness nanoparticle tin-based composite solder through gradual speed-change cooling Download PDFInfo
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- 238000001816 cooling Methods 0.000 title claims abstract description 112
- 229910000679 solder Inorganic materials 0.000 title claims abstract description 111
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 86
- 239000002131 composite material Substances 0.000 title claims abstract description 45
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 34
- 230000008569 process Effects 0.000 title claims abstract description 28
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 46
- 239000000956 alloy Substances 0.000 claims abstract description 46
- 238000005096 rolling process Methods 0.000 claims abstract description 40
- 238000003723 Smelting Methods 0.000 claims abstract description 33
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 230000008859 change Effects 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 229910052718 tin Inorganic materials 0.000 claims description 83
- 239000002826 coolant Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 17
- 238000002844 melting Methods 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 11
- 238000000265 homogenisation Methods 0.000 claims description 9
- 238000005520 cutting process Methods 0.000 claims description 7
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 7
- 230000009467 reduction Effects 0.000 claims description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 6
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 6
- 230000004907 flux Effects 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000005476 soldering Methods 0.000 claims description 5
- 239000012300 argon atmosphere Substances 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 235000013024 sodium fluoride Nutrition 0.000 claims description 3
- 239000011775 sodium fluoride Substances 0.000 claims description 3
- 241001062472 Stokellia anisodon Species 0.000 claims description 2
- 238000005219 brazing Methods 0.000 claims description 2
- 239000000945 filler Substances 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000010891 electric arc Methods 0.000 abstract 1
- 229910006640 β-Sn Inorganic materials 0.000 abstract 1
- 229910006632 β—Sn Inorganic materials 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 9
- 238000002360 preparation method Methods 0.000 description 9
- 230000002787 reinforcement Effects 0.000 description 9
- 239000000126 substance Substances 0.000 description 8
- 238000005266 casting Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000006911 nucleation Effects 0.000 description 6
- 238000010899 nucleation Methods 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 5
- 229910000765 intermetallic Inorganic materials 0.000 description 5
- 210000001787 dendrite Anatomy 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000004781 supercooling Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 229910017482 Cu 6 Sn 5 Inorganic materials 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Abstract
The invention discloses a process for obtaining high-strength high-toughness nanoparticle tin-based composite solder through gradual speed change cooling, and belongs to the technical field of solder alloy production processes. The tin-based solder alloy comprises 46-48.2% of Sn, 0.5-1.5% of Ag, 0.3-0.6% of Cu, 1.3-2% of Ni, 0.5-1% of Si, 0.1-1 Sc and the balance of unavoidable impurities in percentage by mass. The heat treatment process for obtaining the high-strength high-toughness nanoparticle reinforced composite solder by controlling the cooling speed comprises the steps of smelting solder alloy by an electric arc furnace, homogenizing treatment, step-by-step variable-speed cooling and controlled rolling. Finally, the tin-based solder alloy containing Sc nano particles and beta-Sn grains with uniform and fine granularity is obtained, and the purpose of improving the strength and toughness of the tin-based solder alloy is achieved.
Description
Technical Field
The invention relates to a process for obtaining high-strength high-toughness nanoparticle tin-based composite solder through gradual speed change cooling, and belongs to the technical field of solder alloy production processes.
Background
As electronic devices tend to be miniaturized and multifunctional, the requirements for interconnection of solder joints and spaces in microelectronic packages are smaller, and higher requirements are placed on the reliability of the solder joints. The addition of the nano particles can refine the matrix structure of the solder, inhibit the growth of intermetallic compounds (IMCs) and improve the mechanical properties of the solder. Therefore, developing a particle-reinforced lead-free solder to improve the mechanical properties of the solder is a serious difficulty in current research.
The invention patent CN115229384A introduces a preparation method of a nano-particle reinforcement coated silver-based composite solder, wherein nano-reinforcement is coated around silver particles by a molten salt method, and is subjected to melting, ingot casting and pressure processing to obtain the silver solder with uniformly distributed reinforcement, so that the technical difficulties of easy aggregation of reinforcement in a metal solution and the like are solved, but the method needs to be carried out at high temperature, the phase change of a tin-based alloy is easy to occur at high temperature, salt residues are easy to adhere to the surfaces of the nano-particles, and the wear resistance of the silver solder is reduced. The invention patent CN1152769C proposes a preparation method of nano-particle reinforcement tin-based composite solder, the solder is prepared by uniformly mixing the granular tin-lead matrix, the nano-particle reinforcement and neutral soldering flux, stirring for 30-40min, and the solder paste is prepared after melting, and the formed solder joint has very high creep resistance, but the method is easy to cause particle bonding during melting, and reduces the strength of solder alloy. SHEN et al propose to obtain fine dendrites by controlled cooling, the increase in cooling rate decreasing fine Ag 3 Sn particles and primary Ag 3 Surface energy of Sn crystal to make fine Ag 3 Sn particles easily adhere to primary Ag 3 Formation of bulk Ag on Sn crystals 3 Sn IMC。
In summary, the existing process for preparing the nanoparticle composite solder generally adopts melting at high temperature to obtain fine nanoparticles, but has the problems of particle bonding, difficult control of high-temperature phase change and the like. In the invention, from the opposite direction, the concentration gradient is generated by controlling the cooling process to realize strong supercooling, so that the nucleation work of particles is reduced. The invention can effectively avoid the problems of particle bonding, high-temperature phase change and the like existing in the prior preparation of nano particles.
Disclosure of Invention
In order to solve the problems of the existing composite solder, the invention provides a process for obtaining high-strength and high-toughness nanoparticle tin-based composite solder through gradual speed change cooling, and the invention adjusts and controls grain nucleation through gradual speed change cooling and combines with mechanical rolling and other processes, thereby achieving the purpose of improving the reliability of a welding joint, and the specific processing steps are as follows:
(1) Arc melting: sn, ag, cu, ni, si, sc, unavoidable impurities and ammonium chloride soldering flux powder are placed in a smelting furnace, alternating current is applied to smelt under argon atmosphere, and tin-based solder alloy is obtained.
(2) Homogenizing: and (3) cutting the molten tin-based brazing filler metal into cylindrical samples, and sending the cylindrical samples into a muffle furnace for homogenization treatment.
(3) Three-stage variable speed cooling: and (3) putting the tin-based solder treated in the step (2) into DTA equipment to perform three-stage variable-speed cooling in flowing argon atmosphere.
(4) And (3) rolling control: the sample was rolled 5 times by a micro rolling mill, a sample having a thickness of 2mm was rolled into a rectangular sheet having a thickness of 150. Mu.m, the rolling reduction amounts of five times were 10%, 15%, 18%, 23%, 26%, and the total deformation amount was 92%, and oil bath heat preservation was performed after rolling.
(5) And (3) carrying out oil quenching and cooling on the tin-based solder alloy treated in the step (4) to obtain the high-strength and high-toughness nanoparticle tin-based composite solder.
Preferably, the total mass percentage of Sn, ag, cu, ni, si, sc and unavoidable impurities in the step (1) is 100%, wherein the total mass percentage of the unavoidable impurities is 46-48.2% of Sn, 0.5-1.5% of Ag, 0.3-0.6% of Cu, 1.3-2% of Ni, 0.5-1% of Si, 0.1-1% of Sc, and the balance of unavoidable impurities.
Preferably, specific parameters of arc melting in step (1) are: the voltage is 20-40V, the current is 200-300A, the frequency is 50Hz, and the smelting temperature is kept at 232-260 ℃. The vacuum degree of the smelting furnace is 0.1MPa. Electromagnetic stirring is adopted in the smelting process, the stirring frequency is controlled to be 10 min/time, and the process of the step (1) is repeated for 3 times
Preferably, the protective agent in the step (1) is 99.5% industrial grade high-purity ammonium chloride powder produced by Bafos chemical industry.
Preferably, in the step (2), the tin-based solder obtained by melting is cut into cylindrical samples of Φ5mm×2mm.
Preferably, in the step (2), the homogenization temperature is 200-250 ℃, the time is 25-30 h, the homogenization time is strictly controlled, the long-term heat preservation is carried out, the heating speed is as slow as possible, and the heating speed is 2 ℃/h. The temperature rise is too fast, the heat preservation time is too short, the homogenization is incomplete, the grain size of the material is too large, and the overall performance is reduced.
Preferably, specific process parameters of the three-stage variable speed cooling in the step (3) are as follows: primary cooling: the cooling speed is 20K/min, the cooling time is 25min, and the cooling medium is water-cooled; and (3) secondary cooling: the cooling speed is 10K/min, the time is 50min, and the cooling medium is oil-cooled; and (3) three-stage cooling: the cooling speed is 5K/min, the time is 120min, and the cooling medium is air-cooled.
Preferably, in the step (4), a layer of sodium fluoride scaling powder is uniformly smeared on the rolling surface of the plate in each rolling, the temperature of an oil bath is controlled to be between 150 and 250 ℃, and the heat preservation time is controlled to be between 300 and 500 seconds, so as to eliminate residual stress of recrystallized grains generated in the rolling process and further promote grain refinement, and the nanoparticle reinforcement is obtained.
Preferably, the soldering flux in the step (4) is sodium fluoride soldering flux of chemical 1333-83-1 of Wuhan Ji Yesheng.
The principle of the invention is as follows: the essence of the nanoparticle reinforcement obtained by controlled cooling is the in situ generation method. The in-situ generation method is to add or generate reinforcing phase in the solder matrix in advance, and then generate or precipitate nano-scale reinforcing body particles in the composite solder by a mechanical process or a method of controlling cooling speed and the like. For Yu Xiji solder alloy, nucleation work can be reduced by variable-speed cooling, and Cu is greatly improved 6 Sn 5 Can promote intermetallic compounds to form small crystal nucleus; on the other hand, the strong kinetic energy supercooling generated by variable speed cooling causes the actual eutectic point to move towards the high Sn concentration, and the eutectic and hypereutectic solder is condensed along the metastable hypoeutecticThe solid path advances, and the crystal is matched with the eutectic Cu 6 Sn 5 The particles nucleate and adhere around the nascent β -Sn, forming a nanoparticle reinforcement.
The beneficial effects of the invention are that
(1) The nano particle nucleation of intermetallic compound is controlled by step-by-step variable speed cooling, and the nano particle reinforcement composite solder alloy is obtained by combining with controlled rolling, thereby achieving the purpose of improving the strength and toughness of the tin-based solder alloy.
(2) The DTA equipment is adopted to monitor the temperature change in real time so as to control gradual speed change cooling, the nucleation of crystal grains is limited in the cooling process, and the atomic diffusion rate is slowed down to achieve the purpose of grain refinement.
(3) The dendrite is refined by adopting a rolling process to obtain the nano-particles.
(4) The addition of rare earth elements can introduce lattice distortion and generate phase change, so that the mechanical and heat treatment properties of the alloy are improved.
(5) The invention has the advantages of simple operation process and easy implementation for enterprises.
Drawings
FIG. 1 is a schematic drawing of a heat treatment process for preparing nanoparticle reinforced composite solder according to the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited to the above.
Example 1
The chemical compositions of the tin-based composite solder implemented by the invention are shown in table 1.
TABLE 1 example 1 chemical composition of tin-based composite solder (%)
| Sn | Sc | Ag | Cu | Ni | Si | Allowance of |
| 46 | 0.1 | 0.5 | 0.3 | 1.3 | 0.5 | Unavoidable impurities |
The specific preparation process is as follows:
(1) Arc melting: smelting and water-cooling casting are carried out according to the components shown in the table 1 to obtain the tin-based solder alloy with the voltage of 30V, the current of 250A and the frequency of 50Hz, and the smelting temperature is kept at 245 ℃. The vacuum degree of the smelting furnace is 0.1MPa. Electromagnetic stirring is adopted in the smelting process, and the stirring frequency is controlled at 10 min/time, so that the tin-based solder alloy is obtained.
(2) Homogenizing: cutting the molten tin-based solder alloy into cylindrical samples with phi of 5mm multiplied by 2mm, and sending the cylindrical samples into a muffle furnace to heat the cylindrical samples to 200 ℃ for 3h.
(3) Three-stage variable speed cooling: putting the tin-based solder treated in the step (2) into DTA equipment for three-stage variable-speed cooling and primary cooling: the cooling speed is 20K/min, the cooling time is 25min, and the cooling medium is water-cooled; and (3) secondary cooling: the cooling speed is 10K/min, the time is 50min, and the cooling medium is oil-cooled; and (3) three-stage cooling: the cooling speed is 5K/min, the time is 120min, and the cooling medium is air-cooled.
(4) And (3) rolling control: and (3) carrying out 5-pass rolling on the tin-based solder alloy treated in the step (3), wherein the rolling reduction of five times is respectively 10%, 15%, 18%, 23% and 26%, the total deformation is 92%, and carrying out oil bath heat preservation after rolling.
(5) And (3) carrying out oil quenching and cooling on the tin-based solder alloy treated in the step (4) to obtain the high-strength and high-toughness nanoparticle tin-based composite solder.
The grain size of the tin-based composite solder was counted by a metallographic microscope in combination with image analysis software, and the tensile strength and impact toughness of the samples were measured by a universal tester, and the experimental results are shown in table 2.
TABLE 2 test results of grain size, tensile Strength and impact toughness of tin-based composite solder of EXAMPLE 1
| Grain size/nm | Tensile strength/MPa | Impact toughness (J/cm) -2 ) |
| 62 | 118 | 45 |
Example 2
The chemical compositions of the tin-based composite solder implemented by the invention are shown in table 3.
TABLE 3 chemical composition of tin-based composite solder (%)
| Sn | Sc | Ag | Cu | Ni | Si | Allowance of |
| 48.2 | 0.5 | 0.2 | 0.15 | 1 | 0.5 | Unavoidable impurities |
The specific preparation process is as follows:
(1) Arc melting: smelting and water-cooling casting are carried out according to the components shown in the table 3 to obtain the tin-based solder alloy with the voltage of 20V, the current of 200A and the frequency of 50Hz, and the smelting temperature is kept at 232 ℃. The vacuum degree of the smelting furnace is 0.1MPa. Electromagnetic stirring is adopted in the smelting process, and the stirring frequency is controlled at 10 min/time, so that the tin-based solder alloy is obtained.
(2) Homogenizing: cutting the molten tin-based solder alloy into cylindrical samples with phi of 5mm multiplied by 2mm, and sending the cylindrical samples into a muffle furnace to heat to 230 ℃ for 2h.
(3) Three-stage variable speed cooling: putting the tin-based solder treated in the step (2) into DTA equipment for three-stage variable-speed cooling and primary cooling: the cooling speed is 20K/min, the cooling time is 25min, and the cooling medium is water-cooled; and (3) secondary cooling: the cooling speed is 10K/min, the time is 50min, and the cooling medium is oil-cooled; and (3) three-stage cooling: the cooling speed is 5K/min, the time is 120min, and the cooling medium is air-cooled.
(4) And (3) rolling control: and (3) carrying out 5-pass rolling on the tin-based solder alloy treated in the step (3), wherein the rolling reduction of five times is respectively 10%, 15%, 18%, 23% and 26%, the total deformation is 92%, and carrying out oil bath heat preservation after rolling.
(5) And (3) carrying out oil quenching and cooling on the tin-based solder alloy treated in the step (4) to obtain the high-strength and high-toughness nanoparticle tin-based composite solder.
The grain size of the tin-based composite solder was counted by a metallographic microscope in combination with image analysis software, and the tensile strength and impact toughness of the samples were measured by a universal tester, and the experimental results are shown in table 4.
TABLE 4 test results of grain size, tensile Strength, and impact toughness of tin-based composite solder of EXAMPLE 2
| Grain size/nm | Tensile strength/MPa | Impact toughness (J/cm) -2 ) |
| 68 | 110 | 43 |
Example 3
The chemical compositions of the tin-based composite solder implemented by the invention are shown in table 5.
TABLE 5 example 3 chemical composition of tin-based composite solder (%)
| Sn | Sc | Ag | Cu | Ni | Si | Allowance of |
| 47.2 | 1 | 0.4 | 0.1 | 1 | 0.6 | Unavoidable impurities |
The specific preparation process is as follows:
(1) Arc melting: smelting and water-cooling casting are carried out according to the components shown in the table 5 to obtain the tin-based solder alloy with the voltage of 40V, the current of 300A and the frequency of 50Hz, and the smelting temperature is kept at 260 ℃. The vacuum degree of the smelting furnace is 0.1MPa. Electromagnetic stirring is adopted in the smelting process, and the stirring frequency is controlled at 10 min/time, so that the tin-based solder alloy is obtained.
(2) Homogenizing: cutting the molten tin-based solder alloy into cylindrical samples with phi of 5mm multiplied by 2mm, and feeding the cylindrical samples into a muffle furnace to heat the cylindrical samples to 250 ℃ for 5h
(3) Three-stage variable speed cooling: putting the tin-based solder treated in the step (2) into DTA equipment for three-stage variable-speed cooling and primary cooling: the cooling speed is 20K/min, the cooling time is 25min, and the cooling medium is water-cooled; and (3) secondary cooling: the cooling speed is 10K/min, the time is 50min, and the cooling medium is oil-cooled; and (3) three-stage cooling: the cooling speed is 5K/min, the time is 120min, and the cooling medium is air-cooled.
(4) And (3) rolling control: and (3) carrying out 5-pass rolling on the tin-based solder alloy treated in the step (3), wherein the rolling reduction of five times is respectively 10%, 15%, 18%, 23% and 26%, the total deformation is 92%, and carrying out oil bath heat preservation after rolling.
(5) And (3) carrying out oil quenching and cooling on the tin-based solder alloy treated in the step (4) to obtain the high-strength and high-toughness nanoparticle tin-based composite solder.
The grain size of the tin-based composite solder was counted by a metallographic microscope in combination with image analysis software, and the tensile strength and impact toughness of the samples were measured by a universal tester, and the experimental results are shown in table 6.
TABLE 6 test results of grain size, tensile Strength and impact toughness of tin-based composite solder of EXAMPLE 3
| Grain size/nm | Tensile strength/MPa | Impact toughness (J/cm) -2 ) |
| 60 | 121 | 48 |
Comparative example 1
This example differs from example 1 by the fact that no homogenization treatment is carried out, the specific preparation process being as follows:
(1) Arc melting: smelting and water-cooling casting are carried out according to the components shown in the table 1 to obtain the tin-based solder alloy with the voltage of 30V, the current of 250A and the frequency of 50Hz, and the smelting temperature is kept at 245 ℃. The vacuum degree of the smelting furnace is 0.1MPa. Electromagnetic stirring is adopted in the smelting process, and the stirring frequency is controlled at 10 min/time, so that the tin-based solder alloy is obtained. .
(2) Three-stage variable speed cooling: putting the tin-based solder obtained in the step (1) into DTA equipment, performing three-stage variable-speed cooling, and performing primary cooling: the cooling speed is 20K/min, the cooling time is 25min, and the cooling medium is water-cooled; and (3) secondary cooling: the cooling speed is 10K/min, the time is 50min, and the cooling medium is oil-cooled; and (3) three-stage cooling: the cooling speed is 5K/min, the time is 120min, and the cooling medium is air-cooled.
(4) And (3) rolling control: and (3) carrying out 5-pass rolling on the tin-based solder alloy treated in the step (3), wherein the rolling reduction of five times is respectively 10%, 15%, 18%, 23% and 26%, the total deformation is 92%, and carrying out oil bath heat preservation after rolling.
(4) And (3) carrying out oil quenching cooling on the tin-based solder alloy treated in the step (3) to obtain the tin-based composite solder.
The grain size of the sample was counted by a metallographic microscope in combination with image analysis software, and the tensile strength and impact toughness of the sample were measured by a universal tester, and the experimental results are shown in table 7.
TABLE 7 test results of grain size, tensile Strength and impact toughness of tin-based composite solder of comparative example 1
| Grain size/nm | Tensile strength/MPa | Impact toughness (J/cm) -2 ) |
| 68 | 106 | 40 |
Comparative example 2
This example differs from example 2 by replacing the three-stage variable speed cooling with normal cooling, and the specific preparation process is as follows:
(1) Arc melting: smelting and water-cooling casting are carried out according to the components shown in the table 3 to obtain the tin-based solder alloy with the voltage of 20V, the current of 200A and the frequency of 50Hz, and the smelting temperature is kept at 232 ℃. The vacuum degree of the smelting furnace is 0.1MPa. Electromagnetic stirring is adopted in the smelting process, and the stirring frequency is controlled at 10 min/time, so that the tin-based solder alloy is obtained.
(2) Homogenizing: cutting the molten tin-based solder alloy into cylindrical samples with phi of 5mm multiplied by 2mm, and sending the cylindrical samples into a muffle furnace to heat to 230 ℃ for 2h.
(3) And (3) cooling: and (3) putting the tin-based solder treated in the step (2) into a DTA device for cooling, wherein the cooling speed is 10K/min, the cooling time is 50min, and the cooling medium is oil-cooled.
(4) And (3) rolling control: and (3) carrying out 5-pass rolling on the tin-based solder alloy treated in the step (3), wherein the rolling reduction of five times is respectively 10%, 15%, 18%, 23% and 26%, the total deformation is 92%, and carrying out oil bath heat preservation after rolling.
(5) And (3) carrying out oil quenching cooling on the tin-based solder alloy treated in the step (4) to obtain the tin-based composite solder.
The grain size of the tin-based composite solder was counted by a metallographic microscope in combination with image analysis software, and the tensile strength and impact toughness of the samples were measured by a universal tester, and the experimental results are shown in table 8.
Table 8 comparative example 2 tin-based composite solder grain size, tensile Strength, impact toughness test results
| Grain size/nm | Tensile strength/MPa | Impact toughness (J/cm) -2 ) |
| 70 | 101 | 37 |
Comparative example 3
The only difference between this example and example 3 as a comparison is that no controlled rolling is performed, the specific preparation process is as follows:
(1) Arc melting: smelting and water-cooling casting are carried out according to the components shown in the table 5 to obtain the tin-based solder alloy with the voltage of 40V, the current of 300A and the frequency of 50Hz, and the smelting temperature is kept at 260 ℃. The vacuum degree of the smelting furnace is 0.1MPa. Electromagnetic stirring is adopted in the smelting process, and the stirring frequency is controlled at 10 min/time, so that the tin-based solder alloy is obtained.
(2) Homogenizing: cutting the molten tin-based solder alloy into cylindrical samples with phi of 5mm multiplied by 2mm, and sending the cylindrical samples into a muffle furnace to heat to 230 ℃ for 5h.
(3) Three-stage variable speed cooling: putting the tin-based solder treated in the step (2) into DTA equipment for three-stage variable-speed cooling and primary cooling: the cooling speed is 20K/min, the cooling time is 25min, and the cooling medium is water-cooled; and (3) secondary cooling: the cooling speed is 10K/min, the time is 50min, and the cooling medium is oil-cooled; and (3) three-stage cooling: the cooling speed is 5K/min, the time is 120min, and the cooling medium is air-cooled, so that the tin-based composite solder is obtained.
The grain size of the tin-based composite solder was counted by a metallographic microscope in combination with image analysis software, and the tensile strength and impact toughness of the samples were measured by a universal tester, and the experimental results are shown in table 9.
TABLE 9 comparative example 3 grain size, tensile Strength and impact toughness test results of tin-based composite solder
| Grain size/nm | Tensile strength/MPa | Impact toughness (J/cm) -2 ) |
| 63 | 112 | 43 |
From the results shown in tables 2 and 7, since the grain size was large when no homogenization treatment was performed, the fine grain strengthening effect was reduced, and the tensile strength and impact toughness of the solder alloy were both reduced. The reason is that the homogenization treatment can promote the recrystallization and grain boundary migration of the grains and refine the grains.
From the results shown in tables 4 and 8, it can be seen that three-stage variable speed cooling can significantly refine the nanoparticle size, improving the tensile strength and impact toughness of the solder alloy. The reason is that the nucleation work can be reduced by variable speed cooling, and Cu is greatly improved 6 Sn 5 Can promote the formation of small nuclei of intermetallic compounds.
From the results shown in tables 6 and 9, it can be seen that the controlled rolling can refine the nanoparticle size, improving the tensile strength and impact toughness of the solder alloy. The reason is that the rolling can crush coarse dendrites in supercooling to become fine broken grains and refine grains.
Claims (7)
1. A process for obtaining high-strength and high-toughness nanoparticle tin-based composite solder through gradual speed-change cooling is characterized in that: the grains are refined through gradual speed change cooling, and the specific processing steps are as follows:
(1) Arc melting: sn, ag, cu, ni, si, sc, unavoidable impurities and ammonium chloride soldering flux powder are placed in a smelting furnace, alternating current is applied to smelt under argon atmosphere to obtain tin-based solder alloy;
(2) Homogenizing: cutting the molten tin-based brazing filler metal into cylindrical samples, and sending the cylindrical samples into a muffle furnace for homogenization treatment;
(3) Three-stage variable speed cooling: putting the tin-based solder treated in the step (2) into DTA equipment to perform three-stage variable-speed cooling in flowing argon atmosphere;
(4) And (3) rolling control: the sample was rolled 5 times by a micro rolling mill, a sample having a thickness of 2mm was rolled into a rectangular sheet having a thickness of 150. Mu.m, the rolling reduction amounts of five times were 10%, 15%, 18%, 23%, 26%, and the total deformation amount was 92%, and oil bath heat preservation was performed after rolling.
(5) And (3) carrying out oil quenching and cooling on the tin-based solder alloy treated in the step (4) to obtain the high-strength and high-toughness nanoparticle tin-based composite solder.
2. The process for obtaining the high-strength and high-toughness nanoparticle tin-based composite solder by step-by-step variable speed cooling according to claim 1, which is characterized in that: the total mass percentage of Sn, ag, cu, ni, si, sc and unavoidable impurities in the step (1) is 100%, wherein the total mass percentage of the unavoidable impurities is 46-48.2% of Sn, 0.5-1.5% of Ag, 0.3-0.6% of Cu, 1.3-2% of Ni, 0.5-1% of Si, 0.1-1% of Sc, and the balance of unavoidable impurities.
3. The process for obtaining the high-strength and high-toughness nanoparticle tin-based composite solder by step-by-step variable speed cooling according to claim 1, which is characterized in that: the specific parameters of arc melting in the step (1) are as follows: the voltage is 20-40V, the current is 200-300A, the frequency is 50Hz, and the smelting temperature is kept at 232-260 ℃. The vacuum degree of the smelting furnace is 0.1MPa. Electromagnetic stirring is adopted in the smelting process, the stirring frequency is controlled to be 10 min/time, and the process of the step (1) is repeated for 3 times.
4. The process for obtaining the high-strength and high-toughness nanoparticle tin-based composite solder by step-by-step variable speed cooling according to claim 1, which is characterized in that: in the step (2), the molten tin-based solder is cut into cylindrical samples with phi of 5mm multiplied by 2 mm.
5. The process for obtaining the high-strength and high-toughness nanoparticle tin-based composite solder by step-by-step variable speed cooling according to claim 1, which is characterized in that: in the step (2), the homogenization temperature is 200-250 ℃, the time is 25-30 h, and the heating rate is 2 ℃/h.
6. The process for obtaining the high-strength and high-toughness nanoparticle tin-based composite solder by step-by-step variable speed cooling according to claim 1, which is characterized in that: the specific technological parameters of the three-stage variable speed cooling in the step (3) are as follows: primary cooling: the cooling speed is 20K/min, the cooling time is 25min, and the cooling medium is water-cooled; and (3) secondary cooling: the cooling speed is 10K/min, the time is 50min, and the cooling medium is oil-cooled; and (3) three-stage cooling: the cooling speed is 5K/min, the time is 120min, and the cooling medium is air-cooled.
7. The process for obtaining the high-strength and high-toughness nanoparticle tin-based composite solder by step-by-step variable speed cooling according to claim 1, which is characterized in that: and (3) uniformly coating a layer of sodium fluoride scaling powder on the rolling surface of the plate in each rolling step (4), controlling the temperature of an oil bath in a range of 150-250 ℃, and controlling the heat preservation time in a range of 300-500 s.
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