CN110512102B - Preparation method of Sn-Ag-Cu alloy preformed soldering lug - Google Patents

Preparation method of Sn-Ag-Cu alloy preformed soldering lug Download PDF

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Publication number
CN110512102B
CN110512102B CN201910963207.1A CN201910963207A CN110512102B CN 110512102 B CN110512102 B CN 110512102B CN 201910963207 A CN201910963207 A CN 201910963207A CN 110512102 B CN110512102 B CN 110512102B
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rolling
alloy
temperature
soldering lug
reduction
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CN110512102A (en
Inventor
何棋
张家涛
李季
彭巨擘
李才巨
邱家龙
贾元伟
郭绍雄
彭言之
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Yunnan Tin New Material Co ltd
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R & D Center Of Yunnan Tin Industry Group Holdings Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24Selection of soldering or welding materials proper
    • B23K35/26Selection of soldering or welding materials proper with the principal constituent melting at less than 400 degrees C
    • B23K35/262Sn as the principal constituent
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B23MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23KSOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/40Making wire or rods for soldering or welding
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C1/00Making non-ferrous alloys
    • C22C1/02Making non-ferrous alloys by melting
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22CALLOYS
    • C22C13/00Alloys based on tin

Abstract

The invention discloses a preparation method of a Sn-Ag-Cu alloy preformed soldering lug, which adopts NaCl and KCl as protective molten salt to prepare Sn-Ag-Cu alloy; the prepared alloy is rolled, and the rolling process comprises two processes of low-temperature high-speed large reduction and high-temperature low-speed small reduction; the preformed soldering lug produced by the preparation method of the Sn-Ag-Cu alloy preformed soldering lug has the advantages of accurate components, complete shape, high dimensional precision, simple process and high production efficiency, and is suitable for batch production.

Description

Preparation method of Sn-Ag-Cu alloy preformed soldering lug
Technical Field
The invention relates to a microelectronic packaging connecting material, in particular to a preparation method of a Sn-Ag-Cu alloy preformed soldering lug.
Background
The traditional tin-lead (Sn-Pb) solder shows excellent performance in the field of electronic packaging, but the solder contains heavy metal lead, so that the normal metabolism of protein can be inhibited, the nervous system of a human can be damaged, and the human body can be greatly damaged. In addition, lead pollutes the natural environment seriously, so WEEE and ROHS instructions are issued in 2003 in European Union, and 'pollution control and management methods for electronic information products' are issued in 2006 in China, so that the use of lead is limited.
At present, the commonly used lead-free solders are mainly tin (Sn) -based solders, and include some lead-free solders such as gold (Au) -based solders, silver (Ag) -based solders, and indium (In) -based solders that are applied In special fields. In the field of electronic packaging, because soldering flux in the used soldering paste contains solvent, rosin, thickener and a large amount of volatile substances, the soldering flux can generate gas during soldering, and the escape of the gas can form a large amount of cavities, thereby affecting the soldering quality and reducing the service life of electronic components. In addition, flux is prohibited in some precision electronic packaging devices; moreover, such devices cannot be cleaned after the soldering is finished, so that the conventional solder cannot meet the use requirements.
The preformed soldering lug is specially researched and produced aiming at the situation, the soldering flux used by the preformed soldering lug is much less than that in soldering paste, and gas generated during soldering is reduced, so that the voidage is effectively reduced. Residues of the soldering flux after the preformed soldering lug is soldered are few; the soldering flux coating of the preformed soldering lug is not required to be carried out manually; it can also be used for fast and accurate mounting by SMT (surface mount technology) mounting equipment. And the temperature of the equipment does not need to be modified when the reflow soldering process is used for reflow. The preformed sheet can also be precisely controlled in amount and processed into various shapes to achieve good welding effects at minimum cost while meeting welding requirements. Solder pre-forms have been widely used in the field of electronic packaging in recent years.
Sn-Ag-Cu is known to be the lead-free solder alloy with the best comprehensive performance and the widest application at present due to the advantages of low melting point, relatively higher wettability, excellent comprehensive performance and the like. Sn-Ag-Cu is a lead-free solder with great potential to replace Sn-Pb solder. However, there are only reports on the preparation of Sn-Ag-Cu alloy preformed solder pads, and therefore, how to prepare Sn-Ag-Cu alloy preformed solder pads becomes a process which is urgently needed in the industry.
Disclosure of Invention
The invention provides a preparation method of a Sn-Ag-Cu alloy preformed soldering lug, which can effectively solve the problems that the Sn-Ag-Cu alloy is easy to oxidize and difficult to process into a strip when being smelted.
The Sn-Ag-Cu alloy solder comprises, by mass, 1.0-5.0% of Ag, 0.4-0.8% of Cu, and the balance of Sn.
The preparation method comprises the following steps:
(1) weighing NaCl and KCl according to the mass ratio of NaCl to KCl =1: 1-1: 5, and uniformly mixing to prepare a protective molten salt;
(2) putting the uniformly mixed protective molten salt into a crucible for preheating, putting the weighed Sn and Cu into the crucible, heating the crucible until the metal is molten, then preserving the heat for 10-30 min, and stirring the alloy solution once by using a quartz rod every 10min in the heat preservation process;
wherein the addition amount of the protective molten salt is 10-20% of the total mass of Sn and Cu, and the heating and melting temperature of Sn and Cu is 1000-1400 ℃;
(3) adding pre-weighed Ag into a crucible, directly and completely melting the Ag by using the heat of Sn and Cu melts, then preserving the heat for 10-30 min, and stirring the alloy solution once by using a quartz rod every 10 min; pouring the obtained alloy solution into an ingot mold to obtain a Sn-Ag-Cu alloy cast ingot; the thickness of the prepared cast ingot is 5-8 mm;
(4) rolling the Sn-Ag-Cu alloy cast ingot obtained in the step (3) into a thin strip by using a hot rolling mill;
the rolling process of the cast ingot consists of low-temperature high-speed large-reduction rough rolling and high-temperature low-speed small-reduction finish rolling, wherein the reduction of each pass of the rough rolling is kept at 0.5-1.0 mm, the rolling temperature is 70-80 ℃, and the rolling speed is 1.5-2 m/min; the reduction of each pass of finish rolling is kept at 0.05-0.1 mm, the rolling temperature is 90-100 ℃, and the rolling speed is 0.8-1.5 m/min;
(5) annealing the thin strip in the step (4) to improve various structural defects caused in the step, eliminate internal stress, refine grains and prevent the strip from cracking so as to improve the mechanical property of the strip;
(6) and (5) blanking the thin strip annealed in the step (5) through a die to obtain the Sn-Ag-Cu alloy preformed soldering lug.
The NaCl in the step (1) is analytically pure NaCl, and the KCl is analytically pure KCl;
the rolling pressure in the step (4) is less than or equal to 500kg, and the linear speed is controlled to be 0.8-2.0 m/min for hot rolling; and the step (4) comprises rough rolling and finish rolling when rolling is carried out; the rough rolling is to roll an ingot with the thickness of 5-8 mm into a strip with the thickness of 1mm, the reduction of each pass is kept at 0.5-1.0 mm, the rolling temperature is 70-80 ℃, and the rolling speed is 1.5-2 m/min; the finish rolling is rolling when the thickness of the strip is less than 1mm, the reduction of each pass is kept at 0.05-0.1 mm, the rolling temperature is 90-100 ℃, and the rolling speed is 0.8-1.5 m/min.
The final thickness of the rolled strip in the step (4) is 0.3-0.8 mm; the annealing temperature of the thin strip in the step (5) is 110-150 ℃, and the annealing time is 2-5 h.
The shape of the die punched in the step (6) can be any one of a circular ring shape, a circular shape, a square frame shape and other irregular shapes according to different used dies; and (4) recovering the residual materials after blanking, recovering the residual materials, remelting the residual materials, and using the residual materials for subsequent processing.
Compared with the prior art, the invention has the following advantages:
(1) the Sn-Cu melt heat is adopted to melt Ag, so that the smelting time of the metal material is shortened, and meanwhile, the energy can be saved and the production cost of the material can be reduced;
(2) during rolling, low-temperature high-speed rough rolling and high-temperature low-speed fine rolling are adopted, the dynamic recovery and dynamic recrystallization of metal are fully utilized, and the texture phenomenon and stress accumulation of the material after rolling are effectively improved; an annealing process is added before blanking, so that the crystal grains of the material are refined, the cracking of the material is prevented, and the mechanical property of the material is improved;
(3) according to the preparation method of the Sn-Ag-Cu alloy preformed soldering lug, the processed Sn-Ag-Cu soldering lug is accurate in component, complete in shape and excellent in welding performance; the process is simple in procedure and high in production efficiency, and soldering lugs in different shapes and sizes can be produced according to different requirements.
Detailed Description
The technical solution of the present invention will be further described below by preferred embodiments of the present invention. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1: the preparation process of the annular Sn96.5-Ag3.0-Cu0.5 preformed soldering lug comprises the following steps:
(1) weighing 96.5g of Sn, 3.0g of Ag and 0.5g of Cu, and putting for later use;
(2) weighing NaCl and KCl according to the mass ratio of NaCl to KCl =1 to 1, and uniformly mixing to prepare 15g of protective molten salt;
(3) putting the protective molten salt into a crucible for preheating, putting the weighed Sn and Cu into the crucible, heating the crucible to 1400 ℃, preserving the temperature for 30min after the metal is completely melted, and stirring the alloy solution once by using a quartz rod every 10min in the heat preservation process;
(4) adding pre-weighed Ag into a crucible, directly and completely melting the Ag by using the heat of Sn and Cu melts, preserving the heat for 20min, and stirring the alloy solution once by using a quartz rod every 10 min; pouring the obtained alloy solution into an ingot mold to obtain a Sn-Ag-Cu alloy ingot, wherein the thickness of the prepared ingot is 8 mm;
(5) rolling the Sn96.5-Ag3.0-Cu0.5 alloy cast ingot prepared in the step (4) into a strip by using a hot rolling mill, and performing five-pass rough rolling at low temperature, high speed and large reduction, wherein the reduction of each pass is 1mm in thickness after 0.8mm rough rolling, the rolling temperature is 75 ℃, and the rolling speed is 2 m/min; when the rolling reduction is small at a high temperature and a low speed, the precision rolling is carried out for 5 passes, the thickness of the strip after the rolling reduction of each pass is 0.1mm and the precision rolling is 0.5mm, the adopted rolling temperature is 100 ℃, and the rolling speed is 1 m/min;
(6) annealing the strip with the thickness of 0.5mm obtained after rolling in the step (5) at the annealing temperature of 150 ℃ for 2 h;
(7) blanking the strip annealed in the step (6) by using a precision die to obtain a ring-shaped preformed soldering lug with the size of phi (3 +/-0.01) mm of outer diameter, phi (2 +/-0.01) mm of inner diameter and (0.5 +/-0.01) mm of thickness;
(8) and (4) recovering and remelting the residual material left after blanking in the step (7), and using the residual material for subsequent processing.
Example 2: the preparation process of the square shaped Sn95.5-Ag3.7-Cu0.8 preformed soldering lug is as follows:
(1) weighing 95.5g of Sn, 3.7g of Ag and 0.8g of Cu, and putting the materials for later use;
(2) weighing NaCl and KCl according to the mass ratio of NaCl to KCl =1 to 2, and uniformly mixing to prepare 12g of protective molten salt;
(3) preheating protective molten salt in a crucible, putting the weighed Sn and Cu in the crucible, heating the crucible to 1300 ℃, preserving heat for 25min after the metal is completely melted, and stirring the alloy solution once by using a quartz rod every 10min in the heat preservation process;
(4) adding pre-weighed Ag into a crucible, directly and completely melting the Ag by using the heat of Sn and Cu melts, preserving the heat for 15min, and stirring the alloy solution once by using a quartz rod every 10 min; pouring the obtained alloy solution into an ingot mold to obtain a Sn-Ag-Cu alloy ingot, wherein the thickness of the prepared ingot is 6 mm;
(5) rolling the Sn95.5-Ag3.7-Cu0.8 alloy ingot prepared in the step (4) into a strip by using a hot rolling mill, and performing rough rolling for 6 passes at low temperature, high speed and large reduction, wherein the thickness of the strip after the rough rolling for 1mm is 1.2mm, the rolling temperature is 70 ℃, and the rolling speed is 1.5 m/min; when the rolling reduction is small at a high temperature and a low speed, the precision rolling is carried out for 5 passes, the thickness of the strip after the rolling reduction of each pass is 0.08mm, the thickness of the strip is 0.7mm, the adopted rolling temperature is 90 ℃, and the rolling speed is 1.5 m/min;
(6) annealing the strip with the thickness of 0.7mm obtained after rolling in the step (5) at the annealing temperature of 120 ℃ for 4 hours;
(7) blanking the strip annealed in the step (6) by using a precision die to obtain a preformed soldering lug with the outer length and width of (5 +/-0.01) mmX (5 +/-0.01) mm and the inner length and width of (2 +/-0.01) mmX (2 +/-0.01) mm;
(8) and (4) recovering and remelting the residual material left after blanking in the step (7), and using the residual material for subsequent processing.
Example 3: the preparation process of the round shaped Sn97.4-Ag2.0-Cu0.6 preformed soldering lug comprises the following steps:
(1) weighing 97.4g of Sn, 2.0g of Ag and 0.6g of Cu, and putting for later use;
(2) weighing NaCl and KCl according to the mass ratio of NaCl to KCl =1 to 4, and uniformly mixing to prepare 19g of protective molten salt;
(3) putting the protective molten salt into a crucible for preheating, putting the weighed Sn and Cu into the crucible, heating the crucible to 1100 ℃, preserving the heat for 15min after the alloy is completely melted, and stirring the alloy solution once by using a quartz rod every 10min in the heat preservation process;
(4) adding pre-weighed Ag into a crucible, directly and completely melting the Ag by using the heat of Sn and Cu melts, preserving the heat for 25min, and stirring the alloy solution once by using a quartz rod every 10 min; pouring the obtained alloy solution into an ingot mold to obtain a Sn-Ag-Cu alloy cast ingot; the thickness of the prepared cast ingot is 5 mm;
(5) rolling the Sn97.4-Ag2.0-Cu0.6 alloy cast ingot prepared in the step (4) into a strip by using a hot rolling mill, and performing rough rolling for 7 passes at low temperature, high speed and large reduction, wherein the thickness of the strip after the rough rolling for each pass is 0.6mm is 1mm, the rolling temperature is 80 ℃, and the rolling speed is 1.8 m/min; when the rolling reduction is small at a high temperature and a low speed, the precision rolling is carried out for 5 passes, the thickness of the strip after the rolling reduction of each pass is 0.06mm, the thickness of the strip is 0.5mm, the adopted rolling temperature is 95 ℃, and the rolling speed is 0.8 m/min;
(6) annealing the strip with the thickness of 0.5mm obtained after rolling in the step (5) at the annealing temperature of 130 ℃ for 5 hours;
(7) blanking the strip annealed in the step (6) by using a precision die to obtain a ring-shaped preformed soldering lug with the size of phi (3 +/-0.01) mm;
(8) and (4) recovering and remelting the residual material left after blanking in the step (7), and using the residual material for subsequent processing.
Finally, it should be noted that the above mentioned embodiments are only preferred embodiments of the present invention, and are not intended to limit the technical solutions of the present invention, and any equivalent replacement or corresponding modification made on the technical features of the present invention still remains in the protection scope of the present invention.

Claims (6)

1. A preparation method of a Sn-Ag-Cu alloy preformed soldering lug is characterized by comprising the following steps: preheating protective molten salt in a crucible, putting weighed Sn and Cu in the crucible, carrying out heat preservation for 10-30 min after heating and melting, then directly adding weighed Ag into the crucible for melting, carrying out heat preservation for 10-30 min, pouring the prepared alloy solution into an ingot mold to prepare an ingot, rolling the ingot into a thin strip by a hot rolling mill, annealing the rolled thin strip, and then punching the annealed thin strip into a Sn-Ag-Cu alloy preformed soldering lug by a mold;
the protective molten salt is prepared by mixing NaCl and KCl according to the mass ratio of 1: 1-1: 5, and the addition amount of the protective molten salt is 10-20% of the total mass of Sn and Cu;
the rolling process of the cast ingot consists of low-temperature high-speed large-reduction rough rolling and high-temperature low-speed small-reduction finish rolling, wherein the reduction of each pass of the rough rolling is kept at 0.5-1.0 mm, the rolling temperature is 70-80 ℃, and the rolling speed is 1.5-2 m/min; the reduction of each pass of finish rolling is kept at 0.05-0.1 mm, the rolling temperature is 90-100 ℃, and the rolling speed is 0.8-1.5 m/min.
2. The method of making a Sn-Ag-Cu alloy pre-formed solder tab of claim 1, wherein: the mass percentages of metals in the Sn-Ag-Cu alloy preformed soldering lug are 1.0-5.0% of Ag, 0.4-0.8% of Cu and the balance of Sn.
3. The method of making a Sn-Ag-Cu alloy pre-formed solder tab of claim 1, wherein: the heating melting temperature of Sn and Cu is 1000-1400 ℃.
4. The method of making a Sn-Ag-Cu alloy pre-formed solder tab of claim 1, wherein: stirring and mixing intermittently in the alloy heat preservation process.
5. The method of making a Sn-Ag-Cu alloy pre-formed solder tab of claim 1, wherein: the thickness of the prepared cast ingot is 5-8 mm.
6. The method of making a Sn-Ag-Cu alloy pre-formed solder tab of claim 1, wherein: the annealing temperature of the thin strip is 110-150 ℃, and the annealing time is 2-5 h.
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CN112894195A (en) * 2021-04-02 2021-06-04 陕西工业职业技术学院 Low-silver lead-free solder alloy for brazing and preparation method thereof

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