CN110977238B - Nano IMC (internal mold decoration) uniformly-enhanced tin-based solder and preparation method thereof - Google Patents
Nano IMC (internal mold decoration) uniformly-enhanced tin-based solder and preparation method thereof Download PDFInfo
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- CN110977238B CN110977238B CN201911359228.9A CN201911359228A CN110977238B CN 110977238 B CN110977238 B CN 110977238B CN 201911359228 A CN201911359228 A CN 201911359228A CN 110977238 B CN110977238 B CN 110977238B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—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
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Abstract
The invention discloses a nano IMC uniformly-enhanced tin-based solder and a preparation method thereof, wherein the solder comprises the following components: the nano IMC uniformly-enhanced tin-based powder is tin solid solutionCu dispersed in bulk matrix6Sn5、Cu3Sn or Ag3Sn nano IMC powder and Cu dispersed and distributed in SnPb matrix6Sn5、Cu3Sn、Ag3Sn or Ni3Sn4Nano IMC powder, distributed Cu in SAC305 matrix6Sn5、Cu3Sn、Ag3Sn or Ni3Sn4One of powders of nano-IMC. The invention can realize the uniform distribution of nano particles in the solder alloy, ensure the effective reaction of nano metal, nano IMC and the solder alloy matrix, effectively improve the melting point of the solder alloy and obtain uniform texture and high strength of the solder alloy.
Description
Technical Field
The invention belongs to the technical field of electronic packaging micro-interconnection, and relates to a multiple remelting connecting material for high-temperature packaging, three-dimensional packaging, system packaging and multi-module packaging and a preparation method thereof.
Background
The electronic packaging micro-interconnection technology is one of the core technologies for packaging various electronic components, modules and assemblies. With the increasing demand and index of electronic components, modules and assemblies for high power and high density packaging in the electronic industry, the service temperature of the electronic components, sheets, modules and assemblies is also increased, which will provide more rigorous requirements for micro-interconnection materials, however, traditional solder alloys, resin bonding materials and the like are not sufficient for high temperature working environments of electronic components and assemblies with high power and large heat productivity. Therefore, the relatively poor high temperature service performance and creep resistance of the interconnection region have become one of the major bottlenecks that restrict the development of high-density packaging and high-power packaging. In addition, in the application of three-dimensional packaging, system packaging and multi-module packaging, multiple remelting process is involved, brazing filler metal and joints which are connected previously are required not to be remelted in the subsequent remelting process, and higher requirements are provided for connecting materials.
In order to solve the above problems, it is desired to increase the melting point of the solder alloy and the re-melting temperature of the joint, and to improve the strength and creep resistance of the joint, and to use the solder alloy in a multiple re-melting structure and a connection process of high-temperature packaging, three-dimensional packaging and system packaging. However, the above nanoparticle-reinforced solder has the following problems: as shown in figure 1, the welding flux is formed by mixing Sn-based alloy powder with nano-particle metal or nano-IMC powder, adding a welding flux and the like to form a welding paste, and placing the welding paste on a welding part through printing and dripping, wherein the nano-particles float to the surface of Sn-based alloy melt along with the melting of the welding flux and the welding flux in the welding process, so that a welding point is not smooth, the surface is rough, the forming is not good, the joint structure is not uniform, the strength is insufficient, the melting point and the creep resistance of the joint alloy cannot be effectively improved, and the particles and the welding flux alloy are mostly in a separated state.
Disclosure of Invention
Aiming at the problems of the existing nanoparticle reinforced solder, the invention provides a nano IMC uniformly reinforced tin-based solder for multiple remelting connection in high-temperature packaging and three-dimensional packaging and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme:
the first technical scheme is as follows:
a nano IMC uniformly-enhanced tin-based solder comprises the following components: 80-90 wt.% of nano IMC uniformly reinforced tin-based powder, 2-8 wt.% of dispersant for uniformly dispersing micro particles, 2-8 wt.% of binder capable of keeping polymer stable, 2-8 wt.% of thinner for improving printability and fluidity of solder paste, and 2-8 wt.% of flux for improving wettability and removing oxide film, wherein: the nano IMC uniformly-reinforced tin-based powder is Cu dispersed and distributed in a tin solid solution matrix6Sn5、Cu3Sn or Ag3Sn nano IMC powder and Cu dispersed and distributed in SnPb matrix6Sn5、Cu3Sn、Ag3Sn or Ni3Sn4Nano IMC powder, distributed Cu in SAC305 matrix6Sn5、Cu3Sn、Ag3Sn or Ni3Sn4One of a powder of nano-IMC; the dispersing agent is methyl amyl alcohol or triethyl hexyl phosphoric acid, the binder is alpha-terpineol or polyisobutylene, the diluent is terpineol or alcohol, and the soldering flux is polymerized rosin or disproportionated rosin.
A preparation method of the nano IMC uniformly-enhanced tin-based solder comprises the following steps:
the method comprises the following steps: adding metal powder into the molten tin, SnPb or SAC305 alloy, continuously heating to completely dissolve the metal powder into the tin, SnPb or SAC305 alloy to form a tin-metal molten liquid, and keeping the temperature for 5-60 min;
step two: pouring the tin-metal melt into a powder sprayer, spraying the melt liquid into a protective atmosphere (nitrogen or argon), cooling the melt liquid, separating out metal from the solution, forming dispersed nanoscale IMC in the continuously solidified liquid drop, and cooling the liquid drop into nano IMC to uniformly strengthen tin-based powder;
step three: and mixing the nano IMC uniformly-enhanced tin-based powder prepared in the step two with a dispersing agent, a binder, a diluent and a soldering flux to obtain the nano IMC uniformly-enhanced tin-based soldering paste.
The second technical scheme is as follows:
a nano IMC uniformly-enhanced tin-based solder comprises the following components: 1-91 wt.% of nano IMC uniformly reinforced tin-based powder, 2-8 wt.% of dispersant for uniformly dispersing micron particles, 2-8 wt.% of binder capable of keeping polymer stable, 2-8 wt.% of thinner for improving printing property and fluidity of solder paste, 2-8 wt.% of soldering flux for improving wetting property and removing oxide film, and 91-1 wt.% of solder alloy powder, wherein: the nano IMC uniformly-reinforced tin-based powder is Cu dispersed and distributed in a tin solid solution matrix6Sn5、Cu3Sn or Ag3Sn nano IMC powder and Cu dispersed and distributed in SnPb matrix6Sn5、Cu3Sn、Ag3Sn or Ni3Sn4Nano IMC powder, distributed Cu in SAC305 matrix6Sn5、Cu3Sn、Ag3Sn or Ni3Sn4One of a powder of nano-IMC; the solder alloy powder is tin-lead eutectic solder alloy powder, tin-lead-silver eutectic solder alloy powder or lead-free solder alloy powder (such as SnCu eutectic alloy, SAC305 alloy, SnAg alloy or SnBi eutectic alloy and the like); the dispersing agent is methyl amyl alcohol or triethyl hexyl phosphoric acid, the binder is alpha-terpineol or polyisobutylene, the diluent is terpineol or alcohol, and the soldering flux is polymerized rosin or disproportionated rosin.
A preparation method of the nano IMC uniformly-enhanced tin-based solder comprises the following steps:
the method comprises the following steps: adding metal powder into the molten tin, SnPb or SAC305 alloy, continuously heating to completely dissolve the metal powder into the tin, SnPb or SAC305 alloy to form a tin-metal molten liquid, and keeping the temperature for 5-15 min;
step two: pouring the tin-metal melt into a powder sprayer, spraying the melt liquid into a protective atmosphere (nitrogen or argon), cooling the melt liquid, separating out metal from the solution, forming dispersed nanoscale IMC in the continuously solidified liquid drop, and cooling the liquid drop into nano IMC to uniformly strengthen tin-based powder;
step three: and mixing the nano IMC uniformly-enhanced tin-based powder prepared in the step two with solder alloy powder, a dispersing agent, a binder, a diluent and soldering flux to obtain the nano IMC uniformly-enhanced tin-based soldering paste.
Compared with the prior art, the invention has the following advantages:
1. compared with the existing solder added with nano metal, nano IMC (intermetallic compound) and the like to form the nano particle reinforced solder, the nano IMC uniformly reinforced tin-based solder can solve the problems that in the welding process, nano particles float to the surface of Sn-based alloy melt along with the melting of a welding flux and the solder, so that after solidification, a welding point is not smooth, the surface is rough, the forming is not good, a joint structure is not uniform, the strength is insufficient, the melting point and the creep resistance of a joint alloy cannot be effectively improved, and the particle solder and the joint alloy are in a plurality of separated states.
2. The invention can realize the uniform distribution of nano particles in the solder alloy, ensure the effective reaction of nano metal, nano IMC and the solder alloy matrix, effectively improve the melting point of the solder alloy and obtain uniform texture and high strength of the solder alloy.
3. The invention is suitable for multiple remelting structures and connection processes of high-temperature packaging, three-dimensional packaging and system packaging.
Drawings
FIG. 1 is a schematic diagram of a conventional nanoparticle-reinforced solder structure;
FIG. 2 is a schematic view of a nano IMC uniformly enhanced tin-based solder structure;
FIG. 3 is a schematic diagram of a method for preparing a nano IMC uniformly reinforced tin-based solder.
Detailed Description
The technical solutions of the present invention are further described below with reference to the following examples, but the present invention is not limited thereto, and any modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Example 1:
the embodiment provides a method for preparing nano IMC uniformly-enhanced tin-based solder, which comprises the steps of adding copper powder into molten tin to form a tin-copper solution, preparing powder containing certain copper and nano IMC in a tin matrix in a dispersed manner in a protective atmosphere by using a powder spraying machine, and mixing the powder with a dispersing agent, an adhesive and a soldering flux to prepare nano IMC uniformly-enhanced tin-based soldering paste. As shown in fig. 3, the specific implementation steps are as follows:
the method comprises the following steps: melting 1000 g of tin, adding 300 g of copper powder into the molten tin, continuously heating to completely dissolve the copper powder in the tin to obtain a tin-copper solution, and keeping the temperature for 10 minutes;
step two: pouring the tin-copper melt into a powder spraying machine, dripping the sprayed solution into a protective nitrogen atmosphere, cooling the molten drop, separating out copper from the solution, forming dispersed IMCs in the continuously solidified drops, cooling the drops into powder, and dispersing and distributing nano IMCs on a tin substrate containing certain copper powder (figure 2);
step three: and mixing the prepared powder with a proper amount of dispersant methyl amyl alcohol, adhesive alpha-terpineol, diluent terpineol and soldering flux rosin in a mass ratio of 82:4:5:4:5 to obtain the nano IMC uniformly-enhanced tin-based solder.
The use method I comprises the following steps:
(1) printing or dripping on the part to be welded by a conventional method;
(2) heating and welding;
(3) forming a joint, wherein the joint is formed by dispersing and distributing nano IMC particles in a tin-copper solid solution.
The use method II comprises the following steps:
(1) printing or dripping on the part to be welded by a conventional method;
(2) heating, welding and preserving heat for a period of time;
(3) and forming a joint, wherein the joint is formed by distributing large IMCs in the tin-copper solid solution.
Example 2:
this example differs from example 1 in that: and in the third step, mixing the prepared powder with SnCu eutectic solder powder to achieve the purposes of adjusting the ratio of the tin-copper solid solution to the dispersed nano IMC particles and adjusting the welding temperature, adding a proper amount of dispersant methyl amyl alcohol, adhesive alpha-terpineol, diluent terpineol and soldering flux rosin, and mixing in a mass ratio of 50:32:4:5:4:5 to obtain the nano IMC uniformly-reinforced tin-based solder.
The using method comprises the following steps:
(1) printing or dripping on the part to be welded by a conventional method;
(2) heating and welding;
(3) forming a joint, wherein the joint is formed by dispersing and distributing nano IMC particles in a tin-copper solid solution.
Example 3:
this example differs from example 1 in that: and in the third step, mixing the prepared powder with SnPb eutectic solder powder to achieve the purposes of adjusting the proportion of the SnPb eutectic alloy and dispersed nano IMC particles and adjusting the welding temperature, adding a proper amount of dispersant methyl amyl alcohol, adhesive alpha-terpineol, diluent terpineol and scaling powder rosin, and mixing in a mass ratio of 60:22:6:3:5:4 to obtain the nano IMC uniformly-reinforced tin-based solder.
The using method comprises the following steps:
(1) printing or dripping on the part to be welded by a conventional method;
(2) heating and welding;
(3) forming a joint, wherein the joint is formed by dispersing nano IMC particles in the SnPb alloy.
Example 4:
this example differs from example 1 in that: and in the third step, mixing the prepared powder with SAC305 alloy powder to achieve the purposes of adjusting the proportion of SAC305 alloy and dispersed nano IMC particles and adjusting the welding temperature, adding a proper amount of dispersant methyl amyl alcohol, adhesive alpha-terpineol, diluent terpineol and soldering flux rosin, and mixing in a mass ratio of 40:42:4:5:5:4 to obtain the nano IMC uniformly-reinforced tin-based solder.
The using method comprises the following steps:
(1) printing or dripping on the part to be welded by a conventional method;
(2) heating and welding;
(3) forming a joint, wherein the joint is formed by dispersing nano IMC particles in SAC305 alloy.
Example 5:
this example differs from example 1 in that: in the first step, Sn is replaced by SnPb alloy, and copper powder is replaced by silver powder.
Example 6:
this example differs from example 1 in that: in the first step, tin is replaced by SAC305 alloy, and copper powder is replaced by nickel powder.
Example 7:
this example differs from examples 2-4 in that: in the third step, the solder alloy powder is tin-lead eutectic solder alloy powder.
Claims (6)
1. A nano intermetallic compound uniformly reinforced tin-based solder is characterized by comprising the following components: 80-90 wt.% of nano intermetallic compound uniformly-reinforced tin-based powder, 2-8 wt.% of dispersant, 2-8 wt.% of binder, 2-8 wt.% of diluent and 2-8 wt.% of soldering flux, wherein the nano intermetallic compound uniformly-reinforced tin-based powder is Cu dispersed and distributed in a tin solid solution matrix6Sn5、Cu3Sn or Ag3Powder of Sn nano intermetallic compound and Cu dispersed and distributed in SnPb matrix6Sn5、Cu3Sn、Ag3Sn or Ni3Sn4Nano intermetallic compound powder, dispersion distribution Cu in SAC305 matrix6Sn5、Cu3Sn、Ag3Sn or Ni3Sn4Nano-scale intermetallic formationOne of the powders of the compound.
2. The nano intermetallic compound uniformly reinforced tin-based solder according to claim 1, wherein the dispersant is methyl amyl alcohol or triethyl hexyl phosphoric acid, the binder is alpha-terpineol or polyisobutylene, the diluent is terpineol or alcohol, and the flux is polymerized rosin or disproportionated rosin.
3. A method for preparing a nano intermetallic uniformly reinforced tin-based solder according to any of claims 1-2, characterized in that said method comprises the following steps:
the method comprises the following steps: adding metal powder into the molten tin, SnPb or SAC305 alloy, continuously heating to completely dissolve the metal powder into the tin, SnPb or SAC305 alloy to form a tin-metal molten liquid, and keeping the temperature for 5-60 min;
step two: pouring the tin-metal melt into a powder sprayer, spraying the melt liquid into a protective atmosphere, cooling the melt liquid, separating out metal from the solution, forming dispersed nano-scale intermetallic compounds in the continuously solidified liquid drops, and cooling the liquid drops into nano-intermetallic compounds to uniformly reinforce tin-based powder;
step three: and (4) mixing the nano intermetallic compound uniformly-reinforced tin-based powder prepared in the step two with a dispersing agent, a binder, a diluent and a soldering flux to obtain the nano intermetallic compound uniformly-reinforced tin-based soldering paste.
4. A nano intermetallic compound uniformly reinforced tin-based solder is characterized by comprising the following components: 1-91 wt.% of nano intermetallic compound uniformly-reinforced tin-based powder, 2-8 wt.% of dispersant, 2-8 wt.% of binder, 2-8 wt.% of diluent, 2-8 wt.% of soldering flux and 1-91 wt.% of brazing alloy powder, wherein the nano intermetallic compound uniformly-reinforced tin-based powder is Cu alloy powder dispersed and distributed in a tin solid solution matrix6Sn5、Cu3Sn or Ag3Powder of Sn nano intermetallic compound and Cu dispersed and distributed in SnPb matrix6Sn5、Cu3Sn、Ag3Sn or Ni3Sn4Nano intermetallic compound powder, dispersion distribution Cu in SAC305 matrix6Sn5、Cu3Sn、Ag3Sn or Ni3Sn4One of a powder of nano intermetallic compound; the solder alloy powder is tin-lead eutectic solder alloy powder, tin-lead-silver eutectic solder alloy powder or lead-free solder alloy powder; the lead-free solder alloy powder is SnCu eutectic alloy, SAC305 alloy, SnAg alloy or SnBi eutectic alloy.
5. The nano intermetallic compound uniformly reinforced tin-based solder according to claim 4, wherein the dispersant is methyl amyl alcohol or triethyl hexyl phosphoric acid, the binder is alpha-terpineol or polyisobutylene, the diluent is terpineol or alcohol, and the flux is polymerized rosin or disproportionated rosin.
6. A method for preparing a nano intermetallic uniformly reinforced tin-based solder according to any of claims 4 to 5, characterized in that said method comprises the following steps:
the method comprises the following steps: adding metal powder into the molten tin, SnPb or SAC305 alloy, continuously heating to completely dissolve the metal powder into the tin, SnPb or SAC305 alloy to form a tin-metal molten liquid, and keeping the temperature for 5-15 min;
step two: pouring the tin-metal melt into a powder sprayer, spraying the melt liquid into a protective atmosphere, cooling the melt liquid, separating out metal from the solution, forming dispersed nano-scale intermetallic compounds in the continuously solidified liquid drops, and cooling the liquid drops into nano-intermetallic compounds to uniformly reinforce tin-based powder;
step three: and (4) mixing the nano intermetallic compound uniformly-reinforced tin-based powder prepared in the step two with solder alloy powder, a dispersing agent, a binder, a diluent and soldering flux to obtain the nano intermetallic compound uniformly-reinforced tin-based soldering paste.
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| CN114799616B (en) * | 2022-04-28 | 2023-10-20 | 桂林电子科技大学 | High-entropy intermetallic compound material, preparation method thereof and electronic solder |
| CN115945825A (en) * | 2023-01-30 | 2023-04-11 | 昆山百柔新材料技术有限公司 | Slurry, preparation method thereof and packaging method of chip heat dissipation structure |
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| KR101007326B1 (en) * | 2008-08-11 | 2011-01-13 | 삼성전기주식회사 | Alloy Nano Particle of Sn-Cu-Ag, Preparation Method Thereof and Ink or Paste Using The Alloy Nano Particle |
| CN101829859B (en) * | 2010-02-04 | 2012-02-15 | 哈尔滨工业大学 | Preparation method of nano Fe-enhanced low temperature leadless composite soldering paste |
| CN102922177B (en) * | 2012-10-25 | 2014-08-13 | 哈尔滨工业大学 | Nano intermetallic compound soldering paste and preparation method thereof |
| CN104588905A (en) * | 2014-11-27 | 2015-05-06 | 哈尔滨工业大学 | Ag-Cu-Ti/Sn nano-particle soldering paste and preparation method thereof |
| CN104759725B (en) * | 2015-04-17 | 2016-10-05 | 哈尔滨工业大学 | A kind of method using micro/nano level metallic particles filling Sn parent metal to realize electronic building brick High-temperature Packaging |
| CN105081600B (en) * | 2015-07-24 | 2017-07-07 | 深圳市福英达工业技术有限公司 | Tinbase brazing solder of LED chip and preparation method thereof is inverted in encapsulation |
| CN106002000A (en) * | 2016-06-23 | 2016-10-12 | 深圳市唯特偶新材料股份有限公司 | Soldering paste and preparation method thereof |
| CN106736025A (en) * | 2016-12-15 | 2017-05-31 | 江门市盈盛焊接材料科技有限公司 | A kind of middle temperature silverless Cu-base soldering material and preparation method thereof |
| WO2019100445A1 (en) * | 2017-11-22 | 2019-05-31 | 深圳市福英达工业技术有限公司 | Micro/nano particle reinforced composite solder and preparation method therefor |
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