CN116748734A - Water-soluble laser soldering paste and preparation method thereof - Google Patents
Water-soluble laser soldering paste and preparation method thereof Download PDFInfo
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- CN116748734A CN116748734A CN202310708680.1A CN202310708680A CN116748734A CN 116748734 A CN116748734 A CN 116748734A CN 202310708680 A CN202310708680 A CN 202310708680A CN 116748734 A CN116748734 A CN 116748734A
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- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 3
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Abstract
The invention discloses a water-soluble laser soldering paste, which is prepared from 75% of lead-free soldering tin powder and 25% of water-soluble soldering paste by mass percent; the water-soluble soldering paste comprises the following components in parts by weight: 55-70 parts of polyethylene glycol, 10-15 parts of water-soluble thixotropic agent, 3-10 parts of water-soluble active agent, 3-5 parts of organic amine, 10-15 parts of fatty alcohol polyoxyethylene ether and 0.1-0.5 part of defoamer. The raw materials can be used for preparing and producing the soldering paste under the normal temperature condition, so that the active material can be prevented from having activity performance attenuation under the high temperature condition, and the activity of the soldering paste is reserved to the greatest extent; compared with the prior art, the water-soluble laser solder paste achieves the performances of no splashing and tin frying of the conventional laser solder paste and strong wetting ability during welding, and residues after welding can be directly cleaned by clean water, so that the use of an organic solvent is reduced, the production cost of enterprises is reduced, the physical harm to staff is reduced, and the environment protection effect is also achieved.
Description
Technical Field
The invention relates to the technical field of welding, in particular to water-soluble laser solder paste and a preparation method thereof.
Background
Along with the popularization of the intelligent manufacturing age, components adopted in the electronic industry are developed in the miniaturization and microminiaturization directions, and when a photosensitive element, a thermosensitive element, a PCB (printed circuit board) and a flexible circuit board are welded by the traditional surface packaging welding technology, conditions such as off-welding, low welding spot strength, electronic element damage and the like are easily caused. And by adopting the laser welding technology, the welding quality can be improved. Laser welding is increasingly widely applied in the field of small microelectronics due to the characteristics of large penetration, small deformation, high efficiency, small heat affected zone, no pollution of welding spots and the like.
The laser soldering paste is produced by using laser as heat source to heat and melt the soldering paste. The laser solder paste is coated on the bonding pad by a dispensing machine or other modes, and the solder paste is melted and then solidified to form a welding spot by laser heating, so that the operation process is simple. However, since the laser solder paste is different from the conventional surface mount solder paste in that the laser solder paste is composed of small-particle tin powder (the particle size is usually 2-25 um), residues formed by partial tin beads which are not completely melted due to lower heat at the edge of the laser spot effect have the risk of causing short circuit on the circuit board. Because laser solder paste is mainly used in the field of small microelectronics, the space between the solder joints is small, and the risk of short circuit is further increased, the residues need to be cleaned.
However, in the prior art, in order to avoid the phenomena of tin explosion, tin beads, insufficient wettability and the like, a tin paste prepared by taking rosin as a base material is mainly used, for example, a preparation method of the anti-splashing laser tin paste disclosed in patent publication No. CN111451669A adopts a special high-boiling-point additive, so that solvent in a soldering flux is prevented from boiling and splashing when instant energy is concentrated to welding spots, the phenomena of tin beads and tin powder are prevented from being taken out, the soldering flux is composed of rosin, a thixotropic agent, organic acid, organic amine and the high-boiling-point additive, and a special organic cleaning agent is required to be used for cleaning the soldering paste based on the rosin after welding, so that the cleaning agent is harmful to operators and environment for a long time and the production cost is increased.
Disclosure of Invention
In view of the above, the present invention aims at overcoming the disadvantages of the prior art, and its main object is to provide a water-soluble laser solder paste and a preparation method thereof, wherein the prepared solder paste does not splash and fry tin during welding, has strong wetting ability, and achieves the purpose that the residues after laser welding can be directly cleaned with water.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the water-soluble laser soldering paste consists of 75% of lead-free soldering powder and 25% of water-soluble soldering paste in percentage by mass; the water-soluble soldering paste comprises the following components in parts by weight: 55-70 parts of polyethylene glycol, 10-15 parts of water-soluble thixotropic agent, 3-10 parts of water-soluble active agent, 3-5 parts of organic amine, 10-15 parts of fatty alcohol polyoxyethylene ether and 0.1-0.5 part of defoamer.
As a preferable scheme, the lead-free soldering tin powder is SnAgCu series alloy, and the grain size is 2-25 mu m.
As a preferable scheme, the SnAgCu series alloy is Sn96.5Ag3.0Cu0.5, and the grain size is 2-12 μm.
As a preferred embodiment, the polyethylene glycol is prepared by polyaddition of polyethylene oxide with water and has the formula HO (CH) 2 CH 2 O) n H, the molecular weight of polyethylene glycol is 10000-20000.
As a preferable scheme, the polyethylene glycol is one or a mixture of two or more of polyethylene glycol 10000, polyethylene glycol 12000 and polyethylene glycol 15000.
As a preferable scheme, the water-soluble thixotropic agent is one or two or more of hydroxypropyl cellulose, hydroxymethyl cellulose, hydroxypropyl methylcellulose and carboxymethyl cellulose; the water-soluble active agent is one or two or more of malonic acid, glycolic acid, succinic acid, malic acid and citric acid, and the purity is higher than 99%.
As a preferable scheme, the organic amine is one or a mixture of two or more of dodecyl amine, hexadecyl amine and octadecyl amine; the defoaming agent is organic silicon defoaming agent, and the organic silicon defoaming agent is one or two or more of AFE-1410, AFE-7610, AFE-3168 and AFE-0050 produced by Dow chemical company.
As a preferable scheme, the fatty alcohol-polyoxyethylene ether is formed by condensing polyethylene glycol and fatty alcohol, and the molecular formula of the fatty alcohol-polyoxyethylene ether is RO (CH) 2 CH 2 O) n H。
As a preferable scheme, the fatty alcohol-polyoxyethylene ether is one or a mixture of two or more of fatty alcohol-polyoxyethylene ether AEO-12, fatty alcohol-polyoxyethylene ether AEO-13 and fatty alcohol-polyoxyethylene ether AEO-14.
A preparation method of water-soluble laser solder paste comprises the following steps:
(1) The polyethylene glycol, the water-soluble thixotropic agent and the water-soluble active agent are put into a pulverizer according to a certain proportion, pulverized and then added into a stirring reaction pot with a dispersing machine;
(2) Placing the organic amine, the fatty alcohol-polyoxyethylene ether and the defoamer into the stirring reaction kettle in the step (1) to be stirred for more than 30 minutes at the rotating speed of 1200 revolutions per minute to obtain a mixture;
(3) Grinding the mixture obtained in the step (2) by using a three-roller grinder to ensure that the particle size of the mixture is smaller than 5 mu m, and obtaining the water-soluble soldering paste.
(4) And (3) proportionally placing the Sn96.5Ag3.0Cu0.5 leadless soldering tin powder and the water-soluble soldering paste obtained in the step (3) into a vacuum stirring pot for stirring, and obtaining the water-soluble laser soldering paste after uniform stirring.
Compared with the prior art, the invention has obvious advantages and beneficial effects, and in particular, the technical scheme can be as follows:
the preparation method is different from the conventional method for dissolving and stirring at a high temperature of more than 100 ℃, and is used for preparing the soldering paste under the condition of normal temperature, so that the active material can be prevented from having activity performance attenuation under the condition of high temperature, and the activity of the soldering paste is reserved to the greatest extent; compared with the prior art, the water-soluble laser solder paste achieves the performances of no splashing and tin frying of the conventional laser solder paste and strong wetting ability during welding, and residues after welding can be directly cleaned by clean water, so that the use of an organic solvent is reduced, the production cost of enterprises is reduced, the physical harm to staff is reduced, and the environment protection effect is also achieved.
In order to more clearly illustrate the efficacy of the invention, the invention is described in detail below in connection with particular examples:
Detailed Description
The invention discloses a water-soluble laser soldering paste, which consists of 75% of lead-free soldering powder and 25% of water-soluble soldering paste by mass percent; the water-soluble soldering paste comprises the following components in parts by weight: 55-70 parts of polyethylene glycol, 10-15 parts of water-soluble thixotropic agent, 3-10 parts of water-soluble active agent, 3-5 parts of organic amine, 10-15 parts of fatty alcohol polyoxyethylene ether and 0.1-0.5 part of defoamer.
The lead-free soldering tin powder is SnAgCu series alloy with the grain diameter of 2-25 mu m, specifically, the SnAgCu series alloy is Sn96.5Ag3.0Cu0.5 with the grain diameter of 2-12 mu m.
The polyethylene glycol is prepared by polyaddition of polyethylene oxide with water, and has a molecular formula of HO (CH) 2 CH 2 O) n H, the molecular weight of polyethylene glycol is 10000-20000; the polyethylene glycol is one or two or more of polyethylene glycol 10000, polyethylene glycol 12000 and polyethylene glycol 15000; the polyethylene glycol has the function of replacing rosin in the conventional laser solder paste, playing a role of stabilizing paste dispensing and molding, and melting into a layer of oil film during high-temperature welding to prevent the melted tin powder from being oxidized again. Meanwhile, the polyethylene glycol has water solubility, can be dissolved in water after being welded, and is convenient for the subsequent water cleaning process.
The water-soluble thixotropic agent is one or two or more of hydroxypropyl cellulose, hydroxymethyl cellulose, hydroxypropyl methylcellulose and carboxymethyl cellulose; the thixotropic agent is added, polar groups in the structure interact to build a three-dimensional net structure, so that the rheological volume of the soldering paste is increased, the free movement space of the soldering paste is limited, and the viscosity of the soldering paste is increased. When shear force is applied, the three-dimensional network structure is destroyed, intermolecular hydrogen bonds disappear, the viscosity is reduced, when the shear force is removed, the hydrogen bonds are reformed, and the three-dimensional network structure is reestablished, thereby ensuring that good rheological properties can be possessed.
The water-soluble active agent is one or two or more of malonic acid, glycolic acid, succinic acid, malic acid and citric acid, and the purity is higher than 99%; the active agent is easy to dissolve in water, and because the carbon chain segment is short, the higher the specific gravity of carboxyl to the whole molecular mass is, the stronger the acidity is, and the active agent is suitable for short-time laser welding, and can rapidly remove the tin powder oxide film and the oxide film on the surface of the welded surface when the temperature is increased.
The organic amine is one or two or more of dodecyl amine, hexadecyl amine and octadecyl amine; the main function of the organic amine is to neutralize the water-soluble active agent, and the water-soluble active agent has strong activity at normal temperature, which is not beneficial to the preservation and use of the solder paste, so the organic amine is used as an acidity regulator to be added into the soldering flux. The organic amine in the flux reacts with the organic acid and forms an amine salt of the acid amine, which is unstable at room temperature and without a catalyst, and which re-decomposes to the organic acid and the organic amine as the laser welding temperature increases. By utilizing the characteristic, the organic amine can inhibit the carboxyl in the organic acid from representing activity at room temperature, and plays a role in relieving the corrosion of the latter to tin powder. In the process of reflow heating, the carboxyl and amino groups which are decomposed and released again by the acid amine salt can play a role of soldering assistance at the same time.
The fatty alcohol polyoxyethylene ether is prepared by condensing polyethylene glycol and fatty alcohol, and the molecular formula is RO (CH) 2 CH 2 O) n H is formed; the fatty alcohol-polyoxyethylene ether is one or two or more of fatty alcohol-polyoxyethylene ether AEO-12, fatty alcohol-polyoxyethylene ether AEO-13 and fatty alcohol-polyoxyethylene ether AEO-14; because the organic acid and the metal oxide film can generate metal salt in the welding process, the metal salt is difficult to dissolve in water, and the added fatty alcohol-polyoxyethylene ether can be dissolved in the metal salt, and the metal salt has hydrophilicity, so that the metal salt can be finally dissolved in water.
The defoaming agent is an organic silicon defoaming agent and comprises, but is not limited to, a silicone oil type defoaming agent, a silicone ether type defoaming agent and a modified organic silicon polyether defoaming agent, wherein the organic silicon defoaming agent is one or a mixture of two or more of AFE-1410, AFE-7610, AFE-3168 and AFE-0050 produced by Dow chemical company; when the residues after welding are cleaned by water, a large amount of gas enters the liquid, the bubbles formed by the low-density floating are unfavorable for thoroughly cleaning the residues after welding, and the organic silicon defoamer can have a bubble breaking effect on the bubbles, so that the production of the bubbles is reduced, and the cleaning process is finished conveniently.
The invention also discloses a preparation method of the water-soluble laser solder paste, which comprises the following steps:
(1) The polyethylene glycol, the water-soluble thixotropic agent and the water-soluble active agent are put into a pulverizer according to a certain proportion, pulverized and then added into a stirring reaction pot with a dispersing machine.
(2) And (3) putting the organic amine, the fatty alcohol-polyoxyethylene ether and the defoamer into the stirring reaction kettle in the step (1), stirring for more than 30 minutes at the rotating speed of 1200 revolutions per minute, and obtaining a mixture.
(3) Grinding the mixture obtained in the step (2) by using a three-roller grinder to ensure that the particle size of the mixture is smaller than 5 mu m, and obtaining the water-soluble soldering paste.
(4) And (3) proportionally placing the Sn96.5Ag3.0Cu0.5 leadless soldering tin powder and the water-soluble soldering paste obtained in the step (3) into a vacuum stirring pot for stirring, and obtaining the water-soluble laser soldering paste after uniform stirring.
The following description is made with reference to specific examples and comparative examples. The ratios of the raw materials used for the water-soluble flux paste of examples 1 to 6 are shown in Table 1.
TABLE 1
The water-soluble soldering paste prepared in examples 1-6 and Sn96.5Ag3.0Cu0.5 leadless soldering powder are proportionally put into a vacuum stirring pot to be stirred, and the water-soluble laser soldering paste can be prepared after uniform stirring
Comparative example 1:
in comparison with example 1, no ethylenediamine was added, and the other production steps were the same as in example 1.
Comparative example 2:
in comparison with example 2, AFE-1410 and AFE7610 were not added, and the other steps were the same as in example 2.
Comparative example 3:
in comparison with example 3, all the raw materials were mixed by heating and dissolving, cooled and then passed through a three-roll mill, and the other production steps were the same as in example 3.
Performance tests were performed on examples 1 to 6 and comparative examples 1 to 3 below, and the test results are shown in table 2.
TABLE 2
Conclusion(s)
As shown in table 2, the organic amine can enhance wetting, prevent tin paste from drying out in the using process, prolong the service life, and the addition of the defoamer has a gain effect on residual cleaning; the test results show that the water-soluble laser solder paste provided by the invention has the properties of no splashing and tin frying of the conventional laser solder paste and strong wetting ability, and residues after welding can be directly cleaned by clear water, so that the water-soluble laser solder paste is suitable for laser welding.
The testing method comprises the following steps:
the solder pastes prepared in comparative examples 1 to 3 were subjected to a solder paste laser welding test for 8 hours or more with reference to Japanese JIS-Z3284 standard, and the performance of splash tin frying and wetting was observed and recorded, and the performance evaluation criteria of splash tin frying and wetting are shown in Table 3; meanwhile, whether the tin paste is dry or not in 8 hours of continuous use is recorded, and whether residues after welding can be cleaned by water or not.
Here, the laboratory ultrasonic 500W was used to clean the sample with clean water for 10 minutes.
TABLE 3 Table 3
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so any minor modifications, equivalent changes and modifications made to the above embodiments according to the technical principles of the present invention are still within the scope of the technical solutions of the present invention.
Claims (10)
1. A water-soluble laser solder paste, characterized in that: calculated by mass percentage, consists of 75% of lead-free soldering tin powder and 25% of water-soluble soldering paste; the water-soluble soldering paste comprises the following components in parts by weight: 55-70 parts of polyethylene glycol, 10-15 parts of water-soluble thixotropic agent, 3-10 parts of water-soluble active agent, 3-5 parts of organic amine, 10-15 parts of fatty alcohol polyoxyethylene ether and 0.1-0.5 part of defoamer.
2. The water-soluble laser solder paste of claim 1, wherein: the lead-free soldering tin powder is SnAgCu series alloy, and the grain diameter is 2-25 mu m.
3. The water-soluble laser solder paste of claim 2, wherein: the SnAgCu series alloy is Sn96.5Ag3.0Cu0.5, and the grain diameter is 2-12 mu m.
4. The water-soluble laser solder paste of claim 1, wherein: the polyethylene glycol is prepared by polyaddition of polyethylene oxide with water, and has a molecular formula of HO (CH) 2 CH 2 O) n H, the molecular weight of polyethylene glycol is 10000-20000.
5. The water-soluble laser solder paste of claim 4, wherein: the polyethylene glycol is one or two or more of polyethylene glycol 10000, polyethylene glycol 12000 and polyethylene glycol 15000.
6. The water-soluble laser solder paste of claim 1, wherein: the water-soluble thixotropic agent is one or two or more of hydroxypropyl cellulose, hydroxymethyl cellulose, hydroxypropyl methylcellulose and carboxymethyl cellulose; the water-soluble active agent is one or two or more of malonic acid, glycolic acid, succinic acid, malic acid and citric acid, and the purity is higher than 99%.
7. The water-soluble laser solder paste of claim 1, wherein: the organic amine is one or two or more of dodecyl amine, hexadecyl amine and octadecyl amine; the defoaming agent is organic silicon defoaming agent, and the organic silicon defoaming agent is one or two or more of AFE-1410, AFE-7610, AFE-3168 and AFE-0050 produced by Dow chemical company.
8. The water-soluble laser solder paste of claim 1, wherein: the fatty alcohol polyoxyethylene ether is formed by condensing polyethylene glycol and fatty alcohol, and the molecular formula of the fatty alcohol polyoxyethylene ether is RO (CH) 2 CH 2 O) n H。
9. The water-soluble laser solder paste of claim 8, wherein: the fatty alcohol-polyoxyethylene ether is one or a mixture of two or more of fatty alcohol-polyoxyethylene ether AEO-12, fatty alcohol-polyoxyethylene ether AEO-13 and fatty alcohol-polyoxyethylene ether AEO-14.
10. A preparation method of water-soluble laser soldering paste is characterized in that: the method comprises the following steps:
(1) The polyethylene glycol, the water-soluble thixotropic agent and the water-soluble active agent according to the proportion are put into a pulverizer to be pulverized, and the pulverized polyethylene glycol, the water-soluble thixotropic agent and the water-soluble active agent are added into a stirring reaction pot with a dispersing machine;
(2) Placing the organic amine, the fatty alcohol-polyoxyethylene ether and the defoamer according to any one of claims 1-9 into the stirring reaction kettle in the step (1) for stirring for more than 30 minutes at a rotating speed of 1200 revolutions per minute to obtain a mixture;
(3) Grinding the mixture obtained in the step (2) by using a three-roller grinder to ensure that the particle size of the mixture is smaller than 5 mu m, and obtaining the water-soluble soldering paste.
(4) And (3) putting the lead-free soldering tin powder and the water-soluble soldering paste obtained in the step (3) into a vacuum stirring pot according to a proportion, stirring uniformly, and obtaining the water-soluble laser soldering paste.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310708680.1A CN116748734A (en) | 2023-06-15 | 2023-06-15 | Water-soluble laser soldering paste and preparation method thereof |
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