CN113770590A - Antimony-containing soldering tin wire free of soldering flux and preparation method thereof - Google Patents

Antimony-containing soldering tin wire free of soldering flux and preparation method thereof Download PDF

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CN113770590A
CN113770590A CN202111191000.0A CN202111191000A CN113770590A CN 113770590 A CN113770590 A CN 113770590A CN 202111191000 A CN202111191000 A CN 202111191000A CN 113770590 A CN113770590 A CN 113770590A
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component
soldering
antimony
wire
flux
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CN113770590B (en
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黄鲁江
夏杰
赵图强
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Zhejiang Qlg Holdings Co ltd
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Zhejiang Qlg 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
    • B23K35/22Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/36Selection 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
    • 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

Abstract

The invention discloses an antimony-containing soldering-flux-free solder wire and a preparation method thereof, wherein the antimony-containing soldering-flux-free solder wire comprises, by mass, 10% -20% of a first component and 80% -90% of a second component; the first component consists of 40 to 60 percent of dibasic ester and 60 to 40 percent of antimony copper compound powder, and the granularity of the antimony copper compound powder is 0.8 to 1.2 microns; the second component is electrolytic tin with the purity of 99.95 percent. The soldering flux-free solder wire obtained by the invention adopts the main component of the intermetallic compound formed by the soldered joint during the traditional soldering as a part of the solder wire alloy, and is fused with the solder through a certain process, thereby realizing soldering flux-free soldering, ensuring that no residue is left after soldering, having better soldering form and higher soldering strength, and being capable of completely meeting and replacing the traditional rosin-type solder wire. The invention provides a novel material for the electronic welding industry, and the novel material has wider application scene and higher application reliability.

Description

Antimony-containing soldering tin wire free of soldering flux and preparation method thereof
Technical Field
The invention relates to a soldering tin wire without soldering flux used in the technical field of electronic welding production, in particular to a soldering tin wire containing antimony and without soldering flux and a preparation method thereof.
Background
The soldering tin wire is used as a main welding material for assembling in the electronic welding industry, the welding quality and reliability are firstly ensured, and the quality of the soldering tin wire directly influences the service life of an assembled product.
At present, a soldering tin wire used in the electronic industry at home and abroad can complete the soldering process only by assisting a certain soldering flux, the soldering flux is necessary to be arranged inside the soldering tin wire or coated with the soldering flux in the soldering process, and the main components of the soldering flux are rosin-based soldering flux and various organic acid activators. Because of the existence of organic acid activators, the activators are not easy to completely decompose in the high-speed welding process and remain on the surface of a weldment together with rosin, and active ingredients in the residues are easy to chemically react with the weldment or a welding point when meeting a high-temperature or humid environment, so that the welding point is continuously corroded, and the service life of a product is influenced.
Disclosure of Invention
In order to overcome the defects, the invention provides the antimony-containing soldering flux-free solder wire and the preparation method thereof, which can effectively improve the service life and reliability of a welding point or a welding part while ensuring the welding effect.
The technical scheme adopted by the invention for solving the technical problem is as follows: an antimony-containing soldering tin wire free of soldering flux comprises, by mass, 10% -20% of a first component and 80% -90% of a second component; the first component consists of 40-60% of dibasic ester and 60-40% of antimony copper compound powder, and the granularity of the antimony copper compound powder is 0.8-1.2 microns; the second component is electrolytic tin with a purity of 99.95%.
As a further improvement of the invention, the composition of the antimony copper compound at least comprises: cu4Sb、Cu2Sb。
As a further improvement of the invention, the CAS code for the dibasic ester (DBE for short) is 95481-62-2.
The invention also provides a preparation method of the antimony-containing soldering-flux-free solder wire, which comprises the following steps:
step 1, uniformly mixing a material dibasic acid ester (DBE, CAS NO:95481-62-2) in the first component and antimony copper compound powder, heating to 90-105 ℃, and keeping continuously stirring to obtain a first component;
step 2, pouring the uniformly mixed first component into a pressure injection barrel with heat preservation and stirring functions for later use;
step 3, weighing the electrolytic tin in the second component, putting the weighed electrolytic tin into an intermediate frequency heating furnace, keeping the temperature within the range of 380-400 ℃, and continuously stirring for 2 hours to obtain the second component;
step 4, casting the second component into a section to be extruded, and cooling for later use;
step 5, putting the extruded section obtained in the step 4 into an extruder for extrusion, pressing the uniformly mixed first component into a second component through a pressurized and sealed injection barrel, wherein the pressing proportion is controlled to be 10-20% through a flow regulating valve, and the pressing proportion is the mass proportion of the first component and the second component;
and 6, controlling the thickness of the wire diameter of the extruded product through a wire drawing die, and reaching the final required wire diameter to obtain the solder wire finished product without the soldering flux.
The invention has the beneficial effects that: the invention adopts dibasic ester and antimony-copper compound as auxiliary materials of soldering tin wire without soldering flux, the function of the soldering tin wire can replace the traditional rosin soldering flux, the wettability is good in the welding process, and an intermetallic compound layer (namely IMC layer, soldered joint) can be formed in a very short time with tin alloy solder and soldered alloy; the traditional welding process utilizes the function of the soldering flux, under the condition of continuous welding high temperature, the formation of intermetallic compounds is also promoted, and the main component of the formed intermetallic compounds is the antimony copper compound, so that the invention can obviously reduce the welding temperature and reduce the thermal shock of the welding high temperature to components; meanwhile, after welding, the soldered joint has no residues, and the reliability of the soldered joint is effectively improved. The antimony and silver elements added in the invention can effectively improve the heat conductivity and the electric conductivity of the solder and reduce the self-energy consumption of the product. In a word, the formula and the process are simple, and the service life and the reliability of the traditional rosin-type solder wire after welding are improved.
Detailed Description
The technical solution of the present invention will be described in detail with reference to examples.
Example 1:
the antimony-containing soldering tin wire without soldering flux comprises, by mass, 10% of a first component and 90% of a second component.
Weighing 4Kg of dibasic ester and 6Kg of antimony copper compound powder of the first component, wherein the median particle size is 1.0 micron;
weighing 100Kg of electrolytic tin with the purity of the second component being 99.95 percent;
the preparation method comprises the following steps:
step 1, uniformly mixing the material dibasic acid ester and the antimony copper compound powder in the first component, heating to 90-105 ℃, and keeping continuously stirring to obtain a first component;
step 2, pouring the uniformly mixed first component into a pressure injection barrel with heat preservation and stirring functions for later use;
step 3, putting the weighed second component electrolytic tin into an intermediate frequency heating furnace, keeping the temperature within the range of 380-400 ℃, and continuously stirring for 2 hours to obtain a second component;
step 4, casting the second component into a section to be extruded, and cooling for later use;
step 5, putting the extruded section obtained in the step 4 into an extruder for extrusion, pressing the uniformly mixed first component into a second component through a pressurized and sealed injection barrel, wherein the pressing proportion is controlled at 10% through a flow regulating valve, and the pressing proportion is the mass proportion of the first component to the second component;
and 6, controlling the thickness of the wire diameter of the extruded product through a wire drawing die, and finally drawing the wire diameter to be 1.5mm to obtain the sample piece of the antimony-containing soldering-flux-free solder wire to be tested in the application example 1.
Example 2:
the antimony-containing soldering tin wire without soldering flux comprises, by mass, 15% of a first component and 85% of a second component.
Weighing 6Kg of dibasic ester and 9Kg of antimony copper compound powder of the first component, wherein the granularity is 1.0 micron;
weighing 100Kg of electrolytic tin with the purity of the second component being 99.95 percent;
the preparation method comprises the following steps:
step 1, uniformly mixing the material dibasic acid ester and the antimony copper compound powder in the first component, heating to 90-105 ℃, and keeping continuously stirring to obtain a first component;
step 2, pouring the uniformly mixed first component into a pressure injection barrel with heat preservation and stirring functions for later use;
step 3, putting the weighed second component electrolytic tin into an intermediate frequency heating furnace, keeping the temperature within the range of 380-400 ℃, and continuously stirring for 2 hours to obtain a second component;
step 4, casting the second component into a section to be extruded, and cooling for later use;
step 5, putting the extruded section obtained in the step 4 into an extruder for extrusion, pressing the uniformly mixed first component into a second component through a pressurized and sealed injection barrel, wherein the pressing proportion is controlled to be 15% through a flow regulating valve, and the pressing proportion is the mass proportion of the first component to the second component;
and 6, controlling the thickness of the wire diameter of the extruded product through a wire drawing die, and finally drawing the wire diameter to be 1.5mm to obtain the sample piece of the antimony-containing soldering-flux-free solder wire to be tested in the application example 2.
Example 3:
the antimony-containing soldering tin wire without soldering flux comprises, by mass, 20% of a first component and 80% of a second component.
Weighing 8Kg of dibasic ester of the first component and 12Kg of antimony-copper compound powder, wherein the median value of the granularity is 1.0 micron;
weighing 100Kg of electrolytic tin with the purity of the second component being 99.95 percent;
the preparation method comprises the following steps:
step 1, uniformly mixing the material dibasic acid ester and the antimony copper compound powder in the first component, heating to 90-105 ℃, and keeping continuously stirring to obtain a first component;
step 2, pouring the uniformly mixed first component into a pressure injection barrel with heat preservation and stirring functions for later use;
step 3, putting the weighed second component electrolytic tin into an intermediate frequency heating furnace, keeping the temperature within the range of 380-400 ℃, and continuously stirring for 2 hours to obtain a second component;
step 4, casting the second component into a section to be extruded, and cooling for later use;
step 5, putting the extruded section obtained in the step 4 into an extruder for extrusion, pressing the uniformly mixed first component into a second component through a pressurized and sealed injection barrel, wherein the pressing proportion is controlled to be 20% through a flow regulating valve, and the pressing proportion is the mass proportion of the first component to the second component;
and 6, controlling the thickness of the wire diameter of the extruded product through a wire drawing die, and finally drawing the wire diameter to be 1.5mm to obtain the sample of the antimony-containing solder-free solder wire to be tested of the embodiment 3.
The three samples of the above examples were compared with conventional solder wires of "1.5 mm wire diameter of tin-copper (sn0.7cu) and 2.0% rosin content" for solder bonding, in which a brass wire having a wire diameter of 1.0mm was bonded to a T2 copper plate, and then "residual state and dryness after soldering, solder spreading rate and solder bonding strength" were observed and tested, and the test results were shown in table 1:
table 1: examples test data sheet
Figure BDA0003301070360000061
Figure BDA0003301070360000071
According to the experimental data, the soldering flux-free solder wire obtained by the technical scheme of the invention has no residue after welding, is dry and does not stick to chalk powder, and meets the GB/T9491 standard; secondly, the spreading rate of the solder during welding reaches more than 87 percent, meets the standard requirement and has little difference with the traditional rosin soldering wire; finally, in the pull-out test of the solder strength test, the overall strength was all stronger than the conventional solder wire.
The antimony-containing soldering tin wire free of soldering flux is suitable for assembling and welding various electronic components, can meet requirements of copper-based welding pieces and welding pieces with multiple alloy components such as nickel plating, silver plating, gold plating and the like, can produce 0.8-2.5 mm soldering tin wire finished products through diameter of finished products, and is high in application universality.
Therefore, the soldering tin wire without soldering flux obtained by the invention adopts the main component of the intermetallic compound formed by the soldered joint (IMC) in the traditional soldering as a part of the soldering tin wire alloy, and is fused with the soldering tin through a certain process, so that soldering flux-free soldering is realized, the residual after soldering is basically avoided, the soldering form (expansion rate) is better, the soldering strength is higher, and the soldering tin wire can completely meet and replace the traditional rosin soldering tin wire. The invention provides a novel material for the electronic welding industry, and the novel material has wider application scene and higher application reliability.
In a word, the invention has breakthrough of new technology on the basis of reaching the weldability and reliability of the traditional soldering wire. In the application process of a client, the original process is not required to be changed, and a better welding effect is achieved.
In the previous description, numerous specific details were set forth in order to provide a thorough understanding of the present invention. The foregoing description is only a preferred embodiment of the invention, which can be embodied in many different forms than described herein, and therefore the invention is not limited to the specific embodiments disclosed above. And that those skilled in the art may, using the methods and techniques disclosed above, make numerous possible variations and modifications to the disclosed embodiments, or modify equivalents thereof, without departing from the scope of the claimed embodiments. Any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the scope of the technical solution of the present invention.

Claims (4)

1. An antimony-containing soldering tin wire free of soldering flux is characterized in that: according to the mass percentage, the paint comprises 10-20% of a first component and 80-90% of a second component;
the first component consists of 40-60% of dibasic ester and 60-40% of antimony copper compound powder, and the granularity of the antimony copper compound powder is 0.8-1.2 microns; the second component is electrolytic tin with a purity of 99.95%.
2. The antimony-containing solder-free wire as set forth in claim 1, wherein: the antimony copper compound at least comprises the following components: cu4Sb、Cu2Sb。
3. The antimony-containing solder-free wire as set forth in claim 1, wherein: the CAS code for the dibasic ester is 95481-62-2.
4. A method for preparing antimony-containing flux-free solder wire according to any one of claims 1 to 3, comprising the steps of:
step 1, uniformly mixing the material dibasic acid ester and the antimony copper compound powder in the first component, heating to 90-105 ℃, and keeping continuously stirring to obtain a first component;
step 2, pouring the uniformly mixed first component into a pressure injection barrel with heat preservation and stirring functions for later use;
step 3, weighing the electrolytic tin in the second component, putting the weighed electrolytic tin into an intermediate frequency heating furnace, keeping the temperature within the range of 380-400 ℃, and continuously stirring for 2 hours to obtain the second component;
step 4, casting the second component into a section to be extruded, and cooling for later use;
step 5, putting the extruded section obtained in the step 4 into an extruder for extrusion, pressing the uniformly mixed first component into a second component through a pressurized and sealed injection barrel, wherein the pressing proportion is controlled to be 10-20% through a flow regulating valve, and the pressing proportion is the mass proportion of the first component and the second component;
and 6, controlling the thickness of the wire diameter of the extruded product through a wire drawing die, and reaching the final required wire diameter to obtain the solder wire finished product without the soldering flux.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102825401A (en) * 2011-06-14 2012-12-19 鞍钢股份有限公司 Corrosion-resistant flux-cored welding wire used for gas shielded welding
CN104070303A (en) * 2013-03-28 2014-10-01 北京康普锡威科技有限公司 Anti-oxidation high-temperature soft-solder solid wire and manufacturing method thereof
US20150217410A1 (en) * 2012-08-10 2015-08-06 Senjumetal Industry Co., Ltd. High-temperature lead-free solder alloy
CN111098062A (en) * 2020-01-09 2020-05-05 东莞市锡达焊锡制品有限公司 High-temperature lead-containing tin wire and production method thereof
CN112605483A (en) * 2020-11-21 2021-04-06 苏州柯仕达电子材料有限公司 Anti-splashing tin wire for electronic packaging and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102825401A (en) * 2011-06-14 2012-12-19 鞍钢股份有限公司 Corrosion-resistant flux-cored welding wire used for gas shielded welding
US20150217410A1 (en) * 2012-08-10 2015-08-06 Senjumetal Industry Co., Ltd. High-temperature lead-free solder alloy
CN104070303A (en) * 2013-03-28 2014-10-01 北京康普锡威科技有限公司 Anti-oxidation high-temperature soft-solder solid wire and manufacturing method thereof
CN111098062A (en) * 2020-01-09 2020-05-05 东莞市锡达焊锡制品有限公司 High-temperature lead-containing tin wire and production method thereof
CN112605483A (en) * 2020-11-21 2021-04-06 苏州柯仕达电子材料有限公司 Anti-splashing tin wire for electronic packaging and preparation method thereof

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