CN111636083B - Protective agent for preventing high-temperature reflow soldering from tin gathering, and preparation method and use method thereof - Google Patents

Protective agent for preventing high-temperature reflow soldering from tin gathering, and preparation method and use method thereof Download PDF

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Publication number
CN111636083B
CN111636083B CN202010507685.4A CN202010507685A CN111636083B CN 111636083 B CN111636083 B CN 111636083B CN 202010507685 A CN202010507685 A CN 202010507685A CN 111636083 B CN111636083 B CN 111636083B
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protective agent
tin
reflow soldering
product
nonionic surfactant
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CN111636083A (en
Inventor
陈春
张兵
向文胜
赵建龙
朱坤
陆兰
顾群艳
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Jiangsu Aisen Semiconductor Material Co ltd
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Jiangsu Aisen Semiconductor Material Co ltd
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48After-treatment of electroplated surfaces
    • 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
    • B23K1/00Soldering, e.g. brazing, or unsoldering
    • B23K1/012Soldering with the use of hot gas
    • 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
    • B23K1/00Soldering, e.g. brazing, or unsoldering
    • B23K1/20Preliminary treatment of work or areas to be soldered, e.g. in respect of a galvanic coating
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/06Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
    • C23C22/48Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
    • C23C22/58Treatment of other metallic material
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/30Electroplating: Baths therefor from solutions of tin

Abstract

The invention discloses a protective agent for preventing high-temperature reflow soldering tin gathering, a preparation method and a using method thereof, wherein the protective agent comprises 1-3wt% of nonionic surfactant, 2-5wt% of citric acid, 1-2wt% of thiourea and the balance of deionized water. The invention can effectively prevent the tin layer from tin piling, tin gathering and the like in the reflow soldering process; simple process, stable product, safety, environmental protection and convenient use.

Description

Protective agent for preventing high-temperature reflow soldering from tin gathering, and preparation method and use method thereof
[ technical field ] A method for producing a semiconductor device
The invention belongs to the technical field of electroplating, and particularly relates to a protective agent for preventing high-temperature reflow soldering from tin gathering, and a preparation method and a use method thereof.
[ background ] A method for producing a semiconductor device
Because tin has the advantages of corrosion resistance, discoloration resistance, no toxicity, easy soldering, softness, low melting point, good ductility and the like, tin is generally used as a plating material to be plated on the surface of electronic components. After the components of electronic products such as semiconductor packaging, PCB printing, passive components and the like are electroplated with tin, the tin layer is easy to discolor, pile tin and the like due to various factors in the reflow soldering process at a high temperature (265 ℃), so that the electrical property of the product is influenced, and the function failure of the product is caused.
At present, a protective agent for preventing high-temperature reflow soldering discoloration exists in the market, for example, the high-temperature reflow soldering tin layer provided by Jiangsu Aisen semiconductor materials GmbH in CN102776496A is used for preventing discoloration, namely, the preparation method and the use method thereof can effectively prevent the discoloration problem of the tin-plated layer in the high-temperature reflow soldering process. Other companies on the market have a plurality of similar products for preventing high-temperature reflow soldering discoloration, but the problems of tin accumulation and tin shrinkage of a tin layer after high-temperature reflow soldering cannot be solved in the using process, as shown in figure 1.
Therefore, it is necessary to provide a new protective agent for preventing high temperature reflow soldering poly-tin, and a preparation method and a use method thereof to solve the above problems.
[ summary of the invention ]
The invention mainly aims to provide a protective agent for preventing high-temperature reflow soldering from tin gathering, which can effectively prevent tin layer tin stacking and tin shrinking.
The invention realizes the purpose through the following technical scheme: the protective agent for preventing high-temperature reflow soldering of the poly-tin comprises 1-3wt% of nonionic surfactant, 2-5wt% of citric acid, 1-2wt% of thiourea and the balance of deionized water.
Further, the nonionic surfactant is one or more of alkylphenol polyoxyethylene OP-10, fatty alcohol polyoxyethylene AEO-10 and alkyl glycoside APG.
The invention also aims to provide a preparation method of the protective agent for preventing high-temperature reflow soldering of the poly-tin, which comprises the following steps:
1) adding two-thirds of water into a container;
2) under the condition of stirring, adding citric acid in proportion until the citric acid is completely dissolved;
3) under the condition of stirring, proportionally adding thiourea until the thiourea is completely dissolved;
4) under the condition of stirring, adding the nonionic surfactant in proportion until the nonionic surfactant is completely dissolved, and continuously stirring for 10-20 minutes;
5) adding water to required amount, and stirring.
Further, the nonionic surfactant is one or more of alkylphenol polyoxyethylene OP-10, fatty alcohol polyoxyethylene AEO-10 and alkyl glycoside APG.
The invention also aims to provide a using method of the protective agent for preventing high-temperature reflow soldering tin gathering, which comprises the following steps: firstly, diluting the protective agent to 1-2 times, then putting the product into the protective agent, soaking the product for 30-120 seconds, taking the product out, cleaning the product, and drying the product.
Compared with the prior art, the protective agent for preventing high-temperature reflow soldering from tin gathering has the beneficial effects that: by adopting a unique complexing film forming principle, when the tin layer is soaked in the tin layer, a special chelating film layer can be formed on the surface of the tin layer, and when the tin layer is in a reflow soldering process at the high temperature of 265 ℃, the chelating film layer keeps the leveling of the molten tin layer by controlling the surface tension of the tin layer, so that the tin layer is ensured not to generate tin condensation phenomenon; the process is simple and effective, the product is stable, safe and environment-friendly, and the use is convenient.
[ description of the drawings ]
FIG. 1 is a diagram of a product after reflow soldering without using the protective agent of the present invention;
FIG. 2 is a diagram of a product after reflow soldering using the protecting agent of the present invention.
[ detailed description ] embodiments
Example (b):
the embodiment is a protective agent for preventing high-temperature reflow soldering of poly-tin, which comprises 1-3wt% of nonionic surfactant, 2-5wt% of citric acid, 1-2wt% of thiourea and the balance of deionized water.
The nonionic surfactant is one or more of alkylphenol polyoxyethylene OP-10, fatty alcohol polyoxyethylene ether AEO-10 and alkyl glycoside APG.
The preparation method of the protective agent comprises the following steps:
1) adding two-thirds of water into a container;
2) under the condition of stirring, adding citric acid in proportion until the citric acid is completely dissolved;
3) under the condition of stirring, proportionally adding thiourea until the thiourea is completely dissolved;
4) under the condition of stirring, adding the nonionic surfactant in proportion until the nonionic surfactant is completely dissolved, and continuously stirring for 10-20 minutes;
5) adding water to required amount, and stirring.
The using method of the protective agent comprises the following steps: firstly, diluting the protective agent to 1-2 times, then putting the product into the protective agent, soaking the product for 30-120 seconds, taking the product out, cleaning the product, and drying the product.
And (3) performing high-temperature reflow soldering at 265 ℃ by using a reflow soldering machine, reflowing repeatedly for three times, and leveling and plumping the appearance of the tin layer without tin stacking and tin shrinking phenomena as shown in figure 2.
In order to verify the effectiveness of the protective agent in the present embodiment, according to the contents of the components specified in table 1 and the above preparation method and use method, different components of the protective agent for preventing high temperature reflow soldering tin accumulation are obtained, which are examples 1 to 4, and the experimental results are shown in table 1:
TABLE 1 specific experimental parameters for the examples
Figure BDA0002527129930000031
The test results in table 1 show that the protective agent for preventing high-temperature solder reflow from tin accumulation provided by the invention can effectively prevent tin accumulation and tin shrinkage of a tin layer under the condition of high-temperature solder reflow at 265 ℃.
When the product is used, other products are prevented from being brought in as much as possible, hands are washed after operation, workplaces and warehouses are ventilated, and contact with skin or splashing into eyes is avoided as much as possible. In the using process, the solution is supplemented according to analysis, and when the effect is deteriorated, a new preparation groove is recommended to be replaced. After the waste liquid is neutralized by alkali, the waste liquid can be normally discharged to a waste water treatment plant.
What has been described above are merely some of the embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.

Claims (3)

1. The protective agent for preventing high-temperature reflow soldering from tin gathering is characterized in that: it comprises 1-3wt% of nonionic surfactant, 2-5wt% of citric acid, 1-2wt% of thiourea and the balance of deionized water; the nonionic surfactant is alkylphenol polyoxyethylene OP-10.
2. A process for the preparation of the protective agent according to claim 1, characterized in that: which comprises the following steps:
1) adding two-thirds of water into a container;
2) under the condition of stirring, adding citric acid in proportion until the citric acid is completely dissolved;
3) under the condition of stirring, proportionally adding thiourea until the thiourea is completely dissolved;
4) under the condition of stirring, adding the nonionic surfactant in proportion until the nonionic surfactant is completely dissolved, and continuously stirring for 10-20 minutes; the nonionic surfactant is alkylphenol ethoxylates OP-10;
5) adding water to required amount, and stirring.
3. A method of using the protectant of claim 1, comprising the steps of: firstly, diluting the protective agent to 1-2 times, then putting the product into the protective agent, soaking the product for 30-120 seconds, taking the product out, cleaning the product, and drying the product.
CN202010507685.4A 2020-06-05 2020-06-05 Protective agent for preventing high-temperature reflow soldering from tin gathering, and preparation method and use method thereof Active CN111636083B (en)

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CN113943934B (en) * 2021-10-26 2023-10-20 海宁市科泰克金属表面技术有限公司 Tin and nickel coating protective agent for electric element

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CN101234460A (en) * 2007-02-01 2008-08-06 上海化工研究院 Water-solubility dip coating tin scaling powder and preparation thereof
CN101560656A (en) * 2009-04-14 2009-10-21 东莞市中实焊锡有限公司 Lead-free printed circuit board copper surface protecting agent and preparation method thereof
WO2010081833A2 (en) * 2009-01-14 2010-07-22 Atotech Deutschland Gmbh Solution and process for increasing the solderability and corrosion resistance of a metal or metal alloy surface
CN102776496A (en) * 2012-04-20 2012-11-14 昆山艾森半导体材料有限公司 Tin layer anti-blushing agent for high-temperature backflow as well as preparation method and use method of tin layer anti-blushing agent
CN103572276A (en) * 2012-07-25 2014-02-12 天津建发精密机械制造有限公司 Preparation method for novel comprehensive oil-removing rust-removing phosphorizing and passivating treating agent
CN107326413A (en) * 2017-07-04 2017-11-07 苏州道蒙恩电子科技有限公司 A kind of electrotinning fastness inorganic agent and application method
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WO2010081833A2 (en) * 2009-01-14 2010-07-22 Atotech Deutschland Gmbh Solution and process for increasing the solderability and corrosion resistance of a metal or metal alloy surface
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CN103572276A (en) * 2012-07-25 2014-02-12 天津建发精密机械制造有限公司 Preparation method for novel comprehensive oil-removing rust-removing phosphorizing and passivating treating agent
CN107326413A (en) * 2017-07-04 2017-11-07 苏州道蒙恩电子科技有限公司 A kind of electrotinning fastness inorganic agent and application method
CN110230061A (en) * 2019-06-26 2019-09-13 珠海横琴思国科技发展有限公司 A kind of gold and silver surface anti-oxidation Anti- tarnishing protective agent and its preparation method and application
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