CN116275694A - Lead-free solder and preparation method thereof - Google Patents
Lead-free solder and preparation method thereof Download PDFInfo
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- CN116275694A CN116275694A CN202310291494.2A CN202310291494A CN116275694A CN 116275694 A CN116275694 A CN 116275694A CN 202310291494 A CN202310291494 A CN 202310291494A CN 116275694 A CN116275694 A CN 116275694A
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- lead
- free solder
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- nano particles
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- 229910000679 solder Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002105 nanoparticle Substances 0.000 claims abstract description 22
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 6
- 229910052802 copper Inorganic materials 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 229910021389 graphene Inorganic materials 0.000 claims description 19
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000003723 Smelting Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 125000003277 amino group Chemical group 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- 238000005266 casting Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000005476 soldering Methods 0.000 claims 1
- 238000003466 welding Methods 0.000 abstract description 25
- 230000003647 oxidation Effects 0.000 abstract description 7
- 238000007254 oxidation reaction Methods 0.000 abstract description 7
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 229910020888 Sn-Cu Inorganic materials 0.000 description 5
- 229910019204 Sn—Cu Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052718 tin Inorganic materials 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000005219 brazing Methods 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004100 electronic packaging Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- -1 3-aminopropyl triethoxysilane modified nano titanium dioxide Chemical class 0.000 description 1
- 229910017482 Cu 6 Sn 5 Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910000765 intermetallic Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/302—Cu as the principal constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B23K35/22—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
- B23K35/264—Bi 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
- B23K35/22—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
- B23K35/28—Selection of soldering or welding materials proper with the principal constituent melting at less than 950 degrees C
- B23K35/282—Zn 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
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3033—Ni 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
-
- 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
- B23K2101/00—Articles made by soldering, welding or cutting
- B23K2101/36—Electric or electronic devices
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Electric Connection Of Electric Components To Printed Circuits (AREA)
Abstract
The invention discloses a lead-free solder, which comprises the following raw materials in percentage by weight: 0.6 to 0.8 percent of Cu, 0.06 to 0.08 percent of modified nano particles, 0.05 to 0.07 percent of Zn, 0.07 to 0.08 percent of Ni, 2.5 to 3 percent of Bi, 0.02 to 0.025 percent of Ge and the balance of Sn. The invention also discloses a preparation method of the lead-free solder. The invention has good wettability and oxidation resistance, low melting point and firm and reliable welding spot.
Description
Technical Field
The invention relates to the technical field of solders, in particular to a lead-free solder and a preparation method thereof.
Background
The Sn-Cu lead-free solder is widely used because of wide sources of raw materials, low cost and no toxic or side effect. Among them, widely used Sn-0.7Cu lead-free solders are commonly used for electronic packaging. However, as electronic packaging gradually develops toward miniaturization, the size of a welding spot is smaller and smaller, and intermetallic compounds (IMCs for short) are generated at the interface of the micro welding spot in the brazing reaction process, which are key to realizing reliable metallurgical interconnection between the brazing filler metal and the under-bump metal layer. However, the brittle nature of IMC at the interface will reduce the mechanical properties and reliability of the micro-pads, and therefore control over thickness and morphology is required. The wettability and oxidation resistance of the Sn-Cu based lead-free solder still need to be improved, and the high melting point of the Sn-Cu based lead-free solder also limits the range of use of the solder.
Disclosure of Invention
Based on the technical problems in the background technology, the invention provides the lead-free solder and the preparation method thereof, and the lead-free solder has good wettability and oxidation resistance, low melting point and firm and reliable welding spots.
The invention provides a lead-free solder, which comprises the following raw materials in percentage by weight: 0.6 to 0.8 percent of Cu, 0.06 to 0.08 percent of modified nano particles, 0.05 to 0.07 percent of Zn, 0.07 to 0.08 percent of Ni, 2.5 to 3 percent of Bi, 0.02 to 0.025 percent of Ge and the balance of Sn.
Preferably, the raw materials comprise the following components in percentage by weight: 0.7% of Cu, 0.07% of modified nano particles, 0.06% of Zn, 0.075% of Ni, 2.7% of Bi, 0.023% of Ge and the balance of Sn.
Preferably, in the preparation process of the modified nano-particles, uniformly mixing the nano-titanium dioxide grafted with the amino with graphene oxide dispersion liquid, stirring at room temperature for 18-24 hours, and carrying out solid-liquid separation to obtain the modified nano-particles.
The nano material is easy to agglomerate and not easy to disperse in the solder, so that the welding performance of the solder is affected; according to the invention, nano titanium dioxide particles are electrostatically assembled on the surface of graphene, so that the originally folded and agglomerated graphene layer is unfolded, and the titanium dioxide nano particles can be uniformly dispersed on the surface of the graphene, thereby avoiding the problem that the nano particles and the graphene are easy to agglomerate; the nano titanium dioxide assembled on the surface of the graphene can improve the dispersibility of the graphene and the nano titanium dioxide in other metal raw materials, so that the effect of the nano material in the solder can be fully exerted.
The above-mentioned amino group-grafted nano titanium dioxide can be obtained by grafting and modifying nano titanium dioxide with an amino group-containing silane coupling agent, which can be 3-aminopropyl triethoxysilane, etc.
Preferably, in the preparation process of the modified nano-particles, the weight ratio of the nano-titanium dioxide grafted with the amino group to the graphene oxide is 5-8:1.
Preferably, during the preparation of the modified nanoparticles, the pH of the graphene oxide dispersion is = 4.5-5.5.
Preferably, in the preparation process of the modified nanoparticles, the solvent of the graphene oxide dispersion liquid is a mixed liquid of ethanol and water.
Preferably, the welding is followed by ultrasonic treatment.
Preferably, the ultrasonic power is 200-250w, the ultrasonic frequency is 10000-15000Hz, and the ultrasonic time is 20-25s.
After welding, ultrasonic treatment is carried out on the welding spots, and proper ultrasonic parameters are selected, so that grains of the IMC in the welding spots can be further refined, the IMC is promoted to grow and extend towards the middle of the welding spots, and the tissue grains are crushed and dispersed in the middle of the welding spots due to ultrasonic action, so that the firmness of the welding spots is improved.
The invention also provides a preparation method of the lead-free solder, which comprises the following steps: under the protection of inert gas, firstly, sn and Bi are melted, then Ni, cu and Ge are sequentially added for smelting, then Zn is added for smelting after the temperature is reduced to 430-450 ℃, finally modified nano particles are added for uniform mixing, then standing is carried out for 15-20min, and the lead-free solder is obtained through casting.
The lead-free solder can be processed into shapes of welding rods, welding wires, welding chips, welding balls and the like.
The beneficial effects are that:
1. according to the invention, the nano titanium dioxide and the graphene are modified, so that the dispersibility of the nano titanium dioxide and the graphene in the solder is greatly improved;
2. uniformly dispersed nano-dioxideTitanium can be adsorbed on IMC (such as Cu 6 Sn 5 ) The groove of the metal-free solder is firmly connected with the IMC, so that element diffusion between the substrate and the solder is prevented, the probability of forming brittle IMC is reduced, and the firmness of a welding spot is improved; the nano titanium dioxide is matched with proper amount of Zn and Ni to further inhibit the growth of brittle IMC, and the Ni can react with Sn and Zn to be adsorbed on the surfaces of Sn and Zn to further improve the problem that Sn-Cu solder and Zn are easy to oxidize; proper amount of Ge and Ni are added to be matched with each other, so that the problem that Sn-Cu solder and Zn are easy to oxidize is further solved;
3. according to the invention, the melting point of the solder is reduced by adding more Bi, and the Bi and the uniformly dispersed graphene are matched with each other, so that the wettability of the solder can be improved, the welding spot is easy to become brittle due to the fact that the Bi content is too high, the compactness and toughness of the welding spot can be improved by adding the graphene, and the problem of embrittlement of the welding spot caused by high Bi content is avoided; 4. and carrying out ultrasonic treatment on the welded spots after welding, so as to further improve the firmness of the welded spots.
Detailed Description
The technical scheme of the invention is described in detail through specific embodiments.
The formulations of examples 1-3 and comparative examples 1-8 are shown in Table 1.
Table 1 Each group of formulations (in weight percent, balance Sn)
The preparation methods of the above examples 1-3 and comparative examples 1-8 are the same: smelting Sn and Bi in a vacuum smelting furnace under the protection of argon, and then sequentially adding Ni, cu and Ge for smelting; then cooling to 450 ℃, adding Zn for smelting, finally adding modified nano particles, fully stirring and uniformly mixing, standing for 15min, casting, and processing to obtain the lead-free welding wire.
The preparation methods of the modified nanoparticles in the above examples 1 to 3 are the same, and are as follows: adding graphene oxide into ethanol water, performing ultrasonic dispersion uniformly, adjusting pH=4.5-5.5, adding 3-aminopropyl triethoxysilane modified nano titanium dioxide, uniformly mixing, stirring at room temperature for 22 hours, filtering, taking a filter cake, washing and drying to obtain modified nano particles.
The welding wires of examples 1-3 and comparative examples 1-8 were respectively used to weld copper alloys, and then ultrasonic was conducted at 220w and 12000Hz for 25s, and the shear strength of the weld spots was measured by a universal tester.
Wettability was measured according to the method of GB 11364-89.
Static oxidation experiments were performed on the welding wires of examples 1-3 and comparative examples 1-8, respectively, at 270 ℃. 300g of the material was weighed each time and placed in a corundum crucible, which was then placed in a tin bath for experiments. Once every 30min, the slag is scraped and weighed once every 1h, each group of experiments lasts for 10h, and the oxidation resistance of the lead-free solder is evaluated according to the oxidation slag amount. The results are shown in Table 2.
TABLE 2 detection results
As can be seen from Table 1, the solder has good wettability and oxidation resistance and good welding spot firmness by mutually matching the elements and the modified nano particles in a proper proportion.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (8)
1. The lead-free solder is characterized by comprising the following raw materials in percentage by weight: 0.6 to 0.8 percent of Cu, 0.06 to 0.08 percent of modified nano particles, 0.05 to 0.07 percent of Zn, 0.07 to 0.08 percent of Ni, 2.5 to 3 percent of Bi, 0.02 to 0.025 percent of Ge and the balance of Sn.
2. The lead-free solder according to claim 1, wherein in the preparation process of the modified nano particles, nano titanium dioxide grafted with amino groups is uniformly mixed with graphene oxide dispersion liquid, stirred at room temperature for 18-24 hours, and subjected to solid-liquid separation to obtain the modified nano particles.
3. The lead-free solder according to claim 2, wherein the weight ratio of the nano titanium dioxide grafted with the amino group to the graphene oxide is 5-8:1 in the preparation process of the modified nano particles.
4. A lead-free solder according to claim 2 or 3, characterized in that during the preparation of the modified nanoparticles, the pH of the graphene oxide dispersion is = 4.5-5.5.
5. The lead-free solder according to any one of claims 2 to 4, wherein in the preparation of the modified nanoparticles, the solvent of the graphene oxide dispersion is a mixture of ethanol and water.
6. The lead-free solder according to any one of claims 1 to 5, wherein the ultrasonic treatment is performed after soldering.
7. The lead-free solder according to claim 6, wherein the ultrasonic power is 200-250w, the ultrasonic frequency is 10000-15000Hz, and the ultrasonic time is 20-25s.
8. A method for producing the lead-free solder according to any one of claims 1 to 7, comprising the steps of: under the protection of inert gas, firstly, sn and Bi are melted, then Ni, cu and Ge are sequentially added for smelting, then Zn is added for smelting after the temperature is reduced to 430-450 ℃, finally modified nano particles are added for uniform mixing, then standing is carried out for 15-20min, and the lead-free solder is obtained through casting.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310291494.2A CN116275694A (en) | 2023-03-23 | 2023-03-23 | Lead-free solder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310291494.2A CN116275694A (en) | 2023-03-23 | 2023-03-23 | Lead-free solder and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116275694A true CN116275694A (en) | 2023-06-23 |
Family
ID=86779583
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310291494.2A Pending CN116275694A (en) | 2023-03-23 | 2023-03-23 | Lead-free solder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116275694A (en) |
-
2023
- 2023-03-23 CN CN202310291494.2A patent/CN116275694A/en active Pending
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