CN111001963B - Soldering tin wire capable of being welded at low temperature and preparation method thereof - Google Patents

Soldering tin wire capable of being welded at low temperature and preparation method thereof Download PDF

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Publication number
CN111001963B
CN111001963B CN201911376259.5A CN201911376259A CN111001963B CN 111001963 B CN111001963 B CN 111001963B CN 201911376259 A CN201911376259 A CN 201911376259A CN 111001963 B CN111001963 B CN 111001963B
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solder
water
tin
nano material
soldering flux
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CN111001963A (en
Inventor
陈钦
宫梦奇
梁少杰
陈旭
徐华侨
张阳
张义宾
翁若伟
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Eunow Electronic Technology Co ltd Suzhou
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Eunow Electronic Technology Co ltd Suzhou
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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
    • B23K35/264—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
    • B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • B23K35/0227—Rods, wires
    • 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
    • B23K35/36—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest
    • B23K35/3612—Selection of non-metallic compositions, e.g. coatings, fluxes; Selection of soldering or welding materials, conjoint with selection of non-metallic compositions, both selections being of interest with organic compounds as principal constituents
    • B23K35/3613—Polymers, e.g. resins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/40—Making wire or rods for soldering or welding

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Electric Connection Of Electric Components To Printed Circuits (AREA)

Abstract

The invention relates to the technical field of low-temperature welding, in particular to a soldering tin wire capable of being welded at low temperature and a preparation method thereof. The coating comprises the following components in parts by weight: 90-100 parts of solder, 0.1-1 part of nano material and 2-2.5 parts of soldering flux; the solder is a tin-bismuth series alloy. The invention adopts the solder, the nano material and the soldering flux to prepare the soldering tin wire which can be welded at low temperature, and adopts the tin-bismuth series alloy as the solder to realize the low-temperature welding; the introduction of the nano material improves the mechanical property of the solder wire; the soldering flux can remove oxides on the metal surface, simultaneously assists heat conduction to enable the soldering flux to reach a soldering temperature as soon as possible, and can also reduce the surface tension of the solder and improve the wettability of the solder. The solder wire has the advantages of low cost, simple manufacture and good wettability, can be used for welding spots at low temperature, and has high strength, good toughness and high reliability.

Description

Soldering tin wire capable of being welded at low temperature and preparation method thereof
Technical Field
The invention relates to the technical field of low-temperature welding, in particular to a soldering tin wire capable of being welded at low temperature and a preparation method thereof.
Background
The low-temperature welding is welding operation below 183 ℃, and can reduce heat damage to electronic components and save energy consumption. At present, representative materials in the field of low-temperature lead-free solders mainly comprise two types, one is a tin-bismuth series alloy, and the other is a tin-indium series alloy. The Sn-Bi alloy and the Sn-in alloy both have the characteristic of melting point lower than 183 ℃ of the Sn-Pb solder, and can realize the connection and the encapsulation of microelectronic products under the requirement of lower soldering equipment, but because the indium belongs to rare noble metals, the raw material cost of the Sn-in solder product is far higher than that of the Sn-Bi solder product under the condition of the same or similar component content. Bismuth is used as a non-toxic element and has rich resources, and can meet the requirement of raw material input for manufacturing the solder. In addition, the tin-bismuth series alloy also has the advantages of low melting point, good wettability, narrow melting range, high creep resistance and the like.
However, in the tin-bismuth alloy, the brittleness is high due to the presence of bismuth, which causes poor ductility of the solder, reduced mechanical properties, and reduced reliability of the solder joint.
In view of the above problems, the present invention is directed to provide a solder wire capable of being soldered at a low temperature, which can be used for soldering at a low temperature, and has high strength, good toughness and high reliability.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides a solder wire capable of being soldered at a low temperature, comprising the following components in parts by weight: 90-100 parts of solder, 0.1-1 part of nano material and 2-2.5 parts of soldering flux; the solder is a tin-bismuth series alloy.
As a preferred technical scheme, the tin-bismuth series alloy comprises the following components in percentage by weight: sn: 42% -43%, Bi: 57% -58%.
As a preferred technical scheme, the tin-bismuth series alloy comprises the following components in percentage by weight: sn: 42%, Bi: 58 percent.
As a preferable technical scheme, the nanomaterial is surface-modified graphene.
As a preferable technical scheme, the soldering flux comprises 80-95 wt% of rosin, 1-5 wt% of solvent, 6-10 wt% of active agent and 2-5 wt% of auxiliary agent.
In a preferred embodiment, the rosin in the flux is at least one selected from the group consisting of maleated rosin, disproportionated rosin, hydrogenated rosin, polymerized rosin, acid-modified rosin, and acrylic rosin.
As a preferred technical solution, in the soldering flux, the solvent is tetrahydrofurfuryl alcohol and/or terpineol.
In a preferred embodiment, in the soldering flux, the active agent is at least one selected from succinic acid, adipic acid, azelaic acid, suberic acid, amino acids, glycolic acid, ammonium bifluoride, and triethylamine trihydrofluoride salt.
As a preferable technical scheme, in the soldering flux, the auxiliary agent is at least one selected from tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, tert-butyl hydroquinone, benzotriazole, triphenoxy phosphine, alkyl phosphate, liquid rubber and liquid rosin.
In a second aspect of the present invention, a method for preparing a solder wire capable of being soldered at a low temperature is provided, which comprises the following steps:
(A) melting the solder, adding the nano material, fully stirring, and smelting the alloy to prepare a bar blank;
(B) and (C) putting the bar blank obtained in the step (A) and the soldering flux into an extruder, and carrying out extrusion treatment and wire drawing treatment.
Has the advantages that: the invention adopts the solder, the nano material and the soldering flux to prepare the soldering tin wire which can be welded at low temperature, and adopts the tin-bismuth series alloy as the solder to realize the low-temperature welding; the introduction of the nano material improves the mechanical property of the solder wire; the soldering flux can remove oxides on the metal surface, simultaneously assists heat conduction to enable the soldering flux to reach a soldering temperature as soon as possible, and can also reduce the surface tension of the solder and improve the wettability of the solder. The solder wire has the advantages of low cost, simple manufacture and good wettability, can be used for welding spots at low temperature, and has high strength, good toughness and high reliability.
Detailed Description
The technical features in the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, but the scope of protection of the present invention is not limited thereto.
"preferred", "more preferred", and the like, in the present invention, refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
The invention provides a soldering tin wire capable of being welded at low temperature, which comprises the following components in parts by weight: 90-100 parts of solder, 0.1-1 part of nano material and 2-2.5 parts of soldering flux.
In a preferred embodiment, the composition comprises the following components in parts by weight: 94-98 parts of solder, 0.2-0.6 part of nano material and 2-2.4 parts of soldering flux.
In a more preferred embodiment, the following ingredients are included in parts by weight: 96 parts of solder, 0.4 part of nano material and 2.2 parts of soldering flux.
Solder
In a preferred embodiment, the solder is a tin bismuth series alloy.
In a preferred embodiment, the tin-bismuth series alloy comprises the following components in percentage by weight: sn: 42% -43%, Bi: 57% -58%.
In a more preferred embodiment, the tin-bismuth series alloy comprises the following components in weight percent: sn: 42%, Bi: 58 percent.
Nano material
In a preferred embodiment, the nanomaterial is surface-modified graphene.
In a preferred embodiment, the preparation method of the nano material at least comprises the following steps:
(1) placing graphene in a mixed solution composed of concentrated sulfuric acid and concentrated nitric acid, soaking for 30min, and washing with water to be neutral;
(2) placing the graphene obtained in the step (1) in SnCl2HCl and waterThe mixed solution (containing 30g of SnCl per 1L of the mixed solution)250mL HCl) for 30min, and washing with water to neutrality;
(3) placing the graphene obtained in the step (2) in AgNO3And ammonia water (each 1L of the mixed solution contains 0.5g of AgNO)330mL ammonia water) for 30min, and washing with water to neutrality;
(4) placing the graphene obtained in the step (3) in AgNO3Silver plating solution consisting of potassium citrate, glucose, ethanol and water (each 1L of silver plating solution contains 23g of AgNO396g of potassium citrate, 28g of glucose and 45mL of ethanol) for 30min, and washing with water to be neutral.
In a preferred embodiment, in step (1), the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is (1-3): 1.
in a more preferred embodiment, in step (1), the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 2: 1.
in a preferred embodiment, in step (3), the concentration of the aqueous ammonia is 20 wt% to 40 wt%.
In a preferred embodiment, in step (3), the concentration of the aqueous ammonia is 30 wt%.
Graphene (Graphene) is a polymer made of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. The graphene has excellent optical, electrical and mechanical properties, has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like, and is considered to be a revolutionary material in the future.
In a preferred embodiment, in the step (1), the thickness of the graphene is 10 to 30 nm.
In a more preferred embodiment, in step (1), the graphene has a thickness of 20 nm.
The graphene was purchased from Nanjing Xiancheng nanomaterial science and technology Co.
The applicant finds out through a large number of experiments that when the specific tin-bismuth series alloy and nano material are adopted to prepare the solder wire, the strict control is carried outThe prepared solder wire has low melting point and excellent mechanical property. The applicant speculates that possible reasons are: ag on the surface of the nano material can react with Sn in the tin-bismuth series alloy to generate Ag3Sn prevents Sn atoms from diffusing to a reaction interface, and particularly for Sn-Bi series alloys, the Sn-Bi series alloys can effectively inhibit the coarsening of a SnBi phase network structure; at the same time, Ag is added under specific conditions3Sn can be uniformly distributed in a system, nucleation is carried out in an out-of-phase mode, and the bridging effect and the load transfer effect of graphene in the nano material are cooperated, so that the strength and the toughness of a welding spot can be effectively improved.
Soldering flux
Flux (flux) refers to a chemical substance that aids and facilitates the soldering process while providing protection and preventing oxidation reactions during the soldering process.
The metal material is heated in the welding process and is easy to generate oxidation reaction, the soldering flux can remove oxides on the metal surface, meanwhile, the soldering flux can assist heat conduction to enable the soldering flux to reach the welding temperature as soon as possible, the surface tension of the solder can be reduced, and the wetting angle is reduced to improve the wettability.
In a preferred embodiment, the soldering flux comprises 80-95 wt% of rosin, 1-5 wt% of solvent, 6-10 wt% of active agent and 2-5 wt% of auxiliary agent.
In a more preferred embodiment, the soldering flux comprises 86% of rosin, 3% of solvent, 8% of active agent and 3% of auxiliary agent by weight percentage.
In a preferred embodiment, the rosin is selected from at least one of maleated rosin, disproportionated rosin, hydrogenated rosin, polymerized rosin, acid-modified rosin, and acrylic rosin.
In a more preferred embodiment, the rosin is a polymerized rosin.
The CAS number of the polymerized rosin is 65997-05-9.
In a preferred embodiment, the solvent is tetrahydrofurfuryl alcohol and/or terpineol.
In a more preferred embodiment, the solvent is tetrahydrofurfuryl alcohol and terpineol.
In a preferred embodiment, the weight ratio of tetrahydrofurfuryl alcohol to terpineol is 1: (1-2).
In a preferred embodiment, the weight ratio of tetrahydrofurfuryl alcohol to terpineol is 1: 1.5.
the CAS number of the tetrahydrofurfuryl alcohol is 97-99-4.
The CAS number of the terpineol is 10482-56-1.
In a preferred embodiment, the active agent is selected from at least one of succinic acid, adipic acid, azelaic acid, suberic acid, amino acids, glycolic acid, ammonium bifluoride, triethylamine trihydrofluoride salt.
In a more preferred embodiment, the active agent is succinic acid, ammonium bifluoride, triethylamine trihydrofluoride salt.
In a preferred embodiment, the weight ratio of succinic acid, ammonium bifluoride and triethylamine trihydrofluoride is (1.8-2.2): (0.9-1.1): 1.
in a more preferred embodiment, the weight ratio of succinic acid, ammonium bifluoride and triethylamine trihydrofluoride is 2:1: 1.
the CAS number of the triethylamine trihydrofluoride salt is 73602-61-6.
In a preferred embodiment, the auxiliary agent is at least one selected from the group consisting of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tert-butyl hydroquinone, benzotriazole, triphenoxy phosphine, alkyl phosphate, liquid rubber and liquid rosin.
In a more preferred embodiment, the auxiliary agent is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] or benzotriazole.
In a preferred embodiment, the weight ratio of the pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] to the benzotriazole is 1: (1-1.5).
In a more preferred embodiment, the weight ratio of the pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] to the benzotriazole is 1: 1.2.
the CAS number of the tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester is 6683-19-8.
In a preferred embodiment, the preparation method of the soldering flux comprises the following steps: adding rosin into a rosin barrel, setting the temperature in the rosin barrel to be 120 ℃, adding an active agent, an auxiliary agent and a solvent after the rosin is melted, fully stirring, and preserving the temperature for 30min to prepare the soldering flux.
In a second aspect of the present invention, a method for preparing a solder wire capable of being soldered at a low temperature is provided, which comprises the following steps:
(A) melting the solder, adding the nano material, fully stirring, and smelting the alloy to prepare a bar blank;
(B) and (C) putting the bar blank obtained in the step (A) and the soldering flux into an extruder, and carrying out extrusion treatment and wire drawing treatment.
Hereinafter, the present invention will be described in more detail by way of examples, but it should be understood that these examples are merely illustrative and not restrictive.
Examples
Example 1
Embodiment 1 of the present invention provides a solder wire capable of being soldered at a low temperature, which comprises the following components in parts by weight: 96 parts of solder, 0.4 part of nano material and 2.2 parts of soldering flux.
The solder is a tin-bismuth series alloy.
The tin-bismuth series alloy comprises the following components in percentage by weight: sn: 42%, Bi: 58 percent.
The nano material is graphene with a modified surface.
The preparation method of the nano material comprises the following steps:
(1) placing graphene in a mixed solution composed of concentrated sulfuric acid and concentrated nitric acid, soaking for 30min, and washing with water to be neutral;
(2) placing the graphene obtained in the step (1) in SnCl2HCl and water (30 g SnCl per 1L of the mixed solution)250mL HCl) of a reaction mixtureConditioning for 30min, and washing with water to neutrality;
(3) placing the graphene obtained in the step (2) in AgNO3And ammonia water (each 1L of the mixed solution contains 0.5g of AgNO)330mL ammonia water) for 30min, and washing with water to neutrality;
(4) placing the graphene obtained in the step (3) in AgNO3Silver plating solution consisting of potassium citrate, glucose, ethanol and water (each 1L of silver plating solution contains 23g of AgNO396g of potassium citrate, 28g of glucose and 45mL of ethanol) for 30min, and washing with water to be neutral.
In the step (1), the thickness of the graphene is 20 nm.
In the step (1), the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 2: 1.
in the step (3), the concentration of the ammonia water is 30 wt%.
The soldering flux comprises 86% of rosin, 3% of solvent, 8% of active agent and 3% of auxiliary agent by weight percentage.
The rosin is polymerized rosin.
The solvent is tetrahydrofurfuryl alcohol and terpineol.
The weight ratio of the tetrahydrofurfuryl alcohol to the terpineol is 1: 1.5.
the active agent is succinic acid, ammonium bifluoride and triethylamine trihydrofluoride.
The weight ratio of the succinic acid to the ammonium bifluoride to the triethylamine trihydrofluoride is 2:1: 1.
the auxiliary agent is tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and benzotriazole.
The weight ratio of the pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] to the benzotriazole is 1: 1.2.
the preparation method of the soldering flux comprises the following steps: adding rosin into a rosin barrel, setting the temperature in the rosin barrel to be 120 ℃, adding an active agent, an auxiliary agent and a solvent after the rosin is melted, fully stirring, and preserving the temperature for 30min to prepare the soldering flux.
Embodiment 1 of the present invention also provides a method for preparing a solder wire capable of being soldered at a low temperature, including the steps of:
(A) melting the solder, adding the nano material, fully stirring, and smelting the alloy to prepare a bar blank;
(B) and (B) putting the bar blank and the soldering flux obtained in the step (A) into an extruder, and performing extrusion treatment and wire drawing treatment to obtain the solder wire with the diameter of 1 mm.
Example 2
Embodiment 2 of the present invention provides a solder wire capable of being soldered at a low temperature, which comprises the following components in parts by weight: 94 parts of solder, 0.2 part of nano material and 2 parts of soldering flux.
The solder is a tin-bismuth series alloy.
The tin-bismuth series alloy comprises the following components in percentage by weight: sn: 42%, Bi: 58 percent.
The nano material is graphene with a modified surface.
The preparation method of the nano material comprises the following steps:
(1) placing graphene in a mixed solution composed of concentrated sulfuric acid and concentrated nitric acid, soaking for 30min, and washing with water to be neutral;
(2) placing the graphene obtained in the step (1) in SnCl2HCl and water (30 g SnCl per 1L of the mixed solution)250mL HCl) for 30min, and washing with water to neutrality;
(3) placing the graphene obtained in the step (2) in AgNO3And ammonia water (each 1L of the mixed solution contains 0.5g of AgNO)330mL ammonia water) for 30min, and washing with water to neutrality;
(4) placing the graphene obtained in the step (3) in AgNO3Silver plating solution consisting of potassium citrate, glucose, ethanol and water (each 1L of silver plating solution contains 23g of AgNO396g of potassium citrate, 28g of glucose and 45mL of ethanol) for 30min, and washing with water to be neutral.
In the step (1), the thickness of the graphene is 10 nm.
In the step (1), the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 2: 1.
in the step (3), the concentration of the ammonia water is 30 wt%.
The soldering flux comprises 80% of rosin, 5% of solvent, 10% of active agent and 5% of auxiliary agent by weight percentage.
The rosin is polymerized rosin.
The solvent is tetrahydrofurfuryl alcohol and terpineol.
The weight ratio of the tetrahydrofurfuryl alcohol to the terpineol is 1:1.
the active agent is succinic acid, ammonium bifluoride and triethylamine trihydrofluoride.
The weight ratio of the succinic acid to the ammonium bifluoride to the triethylamine trihydrofluoride is 1.8: 0.9: 1.
the auxiliary agent is tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and benzotriazole.
The weight ratio of the pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] to the benzotriazole is 1:1.
the preparation method of the soldering flux comprises the following steps: adding rosin into a rosin barrel, setting the temperature in the rosin barrel to be 120 ℃, adding an active agent, an auxiliary agent and a solvent after the rosin is melted, fully stirring, and preserving the temperature for 30min to prepare the soldering flux.
Embodiment 2 of the present invention further provides a method for preparing a solder wire capable of being soldered at a low temperature, including the steps of:
(A) melting the solder, adding the nano material, fully stirring, and smelting the alloy to prepare a bar blank;
(B) and (B) putting the bar blank and the soldering flux obtained in the step (A) into an extruder, and performing extrusion treatment and wire drawing treatment to obtain the solder wire with the diameter of 1 mm.
Example 3
Embodiment 3 of the present invention provides a solder wire capable of being soldered at a low temperature, which comprises the following components in parts by weight: 98 parts of solder, 0.6 part of nano material and 2.4 parts of soldering flux.
The solder is a tin-bismuth series alloy.
The tin-bismuth series alloy comprises the following components in percentage by weight: sn: 43%, Bi: 57 percent.
The nano material is graphene with a modified surface.
The preparation method of the nano material comprises the following steps:
(1) placing graphene in a mixed solution composed of concentrated sulfuric acid and concentrated nitric acid, soaking for 30min, and washing with water to be neutral;
(2) placing the graphene obtained in the step (1) in SnCl2HCl and water (30 g SnCl per 1L of the mixed solution)250mL HCl) for 30min, and washing with water to neutrality;
(3) placing the graphene obtained in the step (2) in AgNO3And ammonia water (each 1L of the mixed solution contains 0.5g of AgNO)330mL ammonia water) for 30min, and washing with water to neutrality;
(4) placing the graphene obtained in the step (3) in AgNO3Silver plating solution consisting of potassium citrate, glucose, ethanol and water (each 1L of silver plating solution contains 23g of AgNO396g of potassium citrate, 28g of glucose and 45mL of ethanol) for 30min, and washing with water to be neutral.
In the step (1), the thickness of the graphene is 30 nm.
In the step (1), the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is 2: 1.
in the step (3), the concentration of the ammonia water is 30 wt%.
The soldering flux comprises 91% of rosin, 1% of solvent, 6% of active agent and 2% of auxiliary agent by weight percentage.
The rosin is polymerized rosin.
The solvent is tetrahydrofurfuryl alcohol and terpineol.
The weight ratio of the tetrahydrofurfuryl alcohol to the terpineol is 1: 2.
the active agent is succinic acid, ammonium bifluoride and triethylamine trihydrofluoride.
The weight ratio of the succinic acid to the ammonium bifluoride to the triethylamine trihydrofluoride is 2.2: 1.1: 1.
the auxiliary agent is tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and benzotriazole.
The weight ratio of the pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] to the benzotriazole is 1: 1.5.
the preparation method of the soldering flux comprises the following steps: adding rosin into a rosin barrel, setting the temperature in the rosin barrel to be 120 ℃, adding an active agent, an auxiliary agent and a solvent after the rosin is melted, fully stirring, and preserving the temperature for 30min to prepare the soldering flux.
Embodiment 3 of the present invention further provides a method for preparing a solder wire capable of being soldered at a low temperature, including the steps of:
(A) melting the solder, adding the nano material, fully stirring, and smelting the alloy to prepare a bar blank;
(B) and (B) putting the bar blank and the soldering flux obtained in the step (A) into an extruder, and performing extrusion treatment and wire drawing treatment to obtain the solder wire with the diameter of 1 mm.
Example 4
The embodiment 4 of the invention provides a soldering wire capable of being soldered at low temperature and a preparation method thereof, and the specific implementation manner is the same as that of the embodiment 1, except that 90 parts of solder and 0.1 part of nano material are used.
Example 5
The embodiment 5 of the invention provides a soldering wire capable of being soldered at low temperature and a preparation method thereof, and the specific implementation mode is the same as that of the embodiment 1, except that 100 parts of solder and 1 part of nano material are used.
Example 6
Embodiment 6 of the present invention provides a solder wire capable of being soldered at a low temperature, and a method for manufacturing a solder wire capable of being soldered at a low temperature, which is the same as embodiment 1 except that the content of the nanomaterial is replaced with 0.
Example 7
The embodiment 7 of the invention provides a solder wire capable of being soldered at a low temperature and a preparation method of the solder wire capable of being soldered at the low temperature, which is the same as the embodiment 1, except that the nano material is graphene, and the thickness of the graphene is 20nm, which is purchased from Nanjing Xiancheng nano material science and technology Limited company.
Example 8
Embodiment 8 of the present invention provides a solder wire capable of being soldered at a low temperature, and further provides a method for preparing a solder wire capable of being soldered at a low temperature, which is the same as embodiment 1, except that the graphene is 5nm thick and is available from Nanjing Xiancheng nanomaterial science and technology Co.
Example 9
Embodiment 9 of the present invention provides a solder wire capable of being soldered at a low temperature, and further provides a method for preparing a solder wire capable of being soldered at a low temperature, which is the same as embodiment 1, except that the graphene is 40nm thick and is available from Nanjing Xiancheng nanomaterial science and technology Co.
Example 10
Embodiment 10 of the present invention provides a solder wire capable of being soldered at a low temperature, and a method for manufacturing a solder wire capable of being soldered at a low temperature, which is the same as embodiment 1 except that 2 parts of the nanomaterial is substituted.
Performance evaluation
Solder joints were formed by using the solder wires solderable at low temperatures described in examples 1 to 10 in accordance with JIS-Z3197, and mechanical properties of the solder joints were measured, and the results of the tests are shown in Table 1.
Table 1 results of performance testing
Tensile strength (MPa) Elongation (%)
Example 1 69 21
Example 2 51 22
Example 3 61 23
Example 4 55 26
Example 5 71 20
Example 6 58 7
Example 7 63 10
Example 8 67 16
Example 9 49 18
Example 10 65 13
The experimental result shows that the soldering tin wire which can be welded at low temperature and is prepared by the invention has high strength and good toughness of the welding spot and high reliability of the welding spot.
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. The use of some numerical ranges in the claims also includes sub-ranges within their range, and variations in these ranges are also to be construed as being covered by the appended claims where possible.

Claims (4)

1. A soldering tin wire capable of being welded at low temperature is characterized by comprising the following components in parts by weight: 90-100 parts of solder, 0.1-1 part of nano material and 2-2.5 parts of soldering flux; the solder is a tin-bismuth series alloy; the tin-bismuth series alloy comprises the following components in percentage by weight: sn: 42% -43%, Bi: 57% -58%;
the nano material is graphene with a modified surface; the preparation method of the nano material at least comprises the following steps:
(1) placing graphene in a mixed solution composed of concentrated sulfuric acid and concentrated nitric acid, soaking for 30min, and washing with water to be neutral;
(2) placing the graphene obtained in the step (1) in SnCl 2Treating the mixture solution of HCl and water for 30min, and washing the mixture solution to be neutral by using water, wherein each 1L of the mixture solution contains: 30g SnCl 2、50mL HCl；
(3) Placing the graphene obtained in the step (2) in AgNO 3And ammonia water for 30min, and washing the mixture with water to be neutral, wherein each 1L of the mixture contains: 0.5g AgNO 330mL of ammonia water;
(4) placing the graphene obtained in the step (3) in AgNO 3 Treating in silver plating solution composed of potassium citrate, glucose, ethanol and water for 30min, and washing with water to neutrality, wherein each 1L of silver plating solution contains: 23g AgNO 396g of potassium citrate, 28g of glucose and 45mL of ethanol;
in the step (1), the volume ratio of the concentrated sulfuric acid to the concentrated nitric acid is (1-3): 1;
in the step (3), the concentration of the ammonia water is 20 wt% -40 wt%;
the soldering flux comprises 80-95 wt% of rosin, 1-5 wt% of solvent, 6-10 wt% of active agent and 2-5 wt% of auxiliary agent;
the rosin is polymerized rosin;
the active agent is succinic acid, ammonium bifluoride and triethylamine trihydrofluoride, and the weight ratio of the succinic acid to the ammonium bifluoride to the triethylamine trihydrofluoride is 2:1: 1;
the auxiliary agent is pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] and benzotriazole, and the weight ratio of the pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] to the benzotriazole is 1: 1.2.
2. A cryo-solderable solder wire as recited in claim 1, wherein the tin-bismuth series alloy comprises, in weight percent: sn: 42%, Bi: 58 percent.
3. A solder wire as claimed in claim 1, characterized in that in the soldering flux, the solvent is tetrahydrofurfuryl alcohol and/or terpineol.
4. A method for preparing a solder wire capable of being soldered as claimed in any of claims 1 to 3, characterized in that it comprises the following steps:
(A) melting the solder, adding the nano material, fully stirring, and smelting the alloy to prepare a bar blank;
(B) and (C) putting the bar blank obtained in the step (A) and the soldering flux into an extruder, and carrying out extrusion treatment and wire drawing treatment.
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