CN115070260A - High-performance tin soldering rod and preparation method thereof - Google Patents
High-performance tin soldering rod and preparation method thereof Download PDFInfo
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- CN115070260A CN115070260A CN202210771302.3A CN202210771302A CN115070260A CN 115070260 A CN115070260 A CN 115070260A CN 202210771302 A CN202210771302 A CN 202210771302A CN 115070260 A CN115070260 A CN 115070260A
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- 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
- B23K35/362—Selection of compositions of fluxes
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- 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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Abstract
The application relates to a high-performance tin soldering rod, which comprises a hollow tin alloy and soldering flux filled in the tin alloy, wherein the soldering flux comprises the following raw materials in percentage by mass: 10-12% of o-iodobenzoic acid, 2-4% of tetrahydrofurfuryl alcohol, 0.6-0.8% of surfactant, 1-2% of triphenylphosphine oxide, 0.1-0.2% of defoaming agent and the balance of rosin. This application has improved the performance of preventing splashing of tin welding stick through adding the defoaming agent in to the scaling powder.
Description
Technical Field
The application relates to the technical field of tin soldering rods, in particular to a high-performance tin soldering rod and a preparation method thereof.
Background
The solder wire is mainly used as a filler metal or a metal wire welding material for electric conduction during welding, and can be classified into rosin type, no-clean type, nickel-plated type, welding type, solid core type and the like. Wherein, rosin type solder wire is with the help of the promotion effect that rosin flows to the molten solder, makes the molten solder flow more easily and the contact is welded the metal, also can prevent to a certain extent by welding the metal surface oxidation phenomenon that appears, and the scaling powder can melt and boil all the time when the solder wire high temperature welding, decomposes the atmospheric pressure that produces great pressure, forms a quantitative high-pressure bubble, and the burst of bubble can cause not little splashing to lead to the fact certain injury to the staff.
In view of the above problems, the inventors thought it necessary to develop a solder bar having spatter-proof properties.
Disclosure of Invention
In order to improve the anti-splashing capacity of the soldering tin rod, the application provides the high-performance soldering tin rod and the preparation method thereof.
The application provides a high-performance tin soldering rod and a preparation method thereof, and the technical scheme is as follows:
a high-performance tin soldering rod comprises a hollow tin alloy and a soldering flux filled in the tin alloy, wherein the soldering flux comprises the following raw materials in percentage by mass: 10-12% of o-iodobenzoic acid, 2-4% of tetrahydrofurfuryl alcohol, 0.6-0.8% of surfactant, 1-2% of triphenylphosphine oxide, 0.1-0.2% of defoaming agent and the balance of rosin.
The o-iodobenzoic acid can remove oxides on the surfaces of the solder and the base material, so that the solder is contacted with the pure base material, and the wetting is effectively finished; the tetrahydrofurfuryl alcohol contributes to a polar environment provided during welding, so that H ions in the active agent are ionized to exert activity; the surface active agent can reduce the surface tension of the liquid soldering flux, so that the soldering flux can smoothly spread on the surface of the base material to remove an oxide film on the surface of the base material, and can reduce the surface tension of the solder and enhance the wetting capacity of the solder to the base material; the triphenylphosphine oxide can form a layer of film on the surface of the substrate so as to play a role in protection and improve the corrosivity remained after welding; the rosin has film forming property, can protect a welding part from being oxidized at high temperature in welding, and a hydrophobic protective film formed after welding has excellent electrical insulation property; the defoaming agent can reduce the splashing phenomenon in the welding process, thereby reducing the damage to workers.
Preferably, the defoaming agent is prepared by adopting the following steps:
(1) mixing octamethylcyclotetrasiloxane and white carbon black, adding NaOH for heating reaction, and cooling after the reaction is finished to prepare hydrophobic white carbon black;
(2) mixing the dimethyl silicone oil and the hydrophobic white carbon black, stirring until the mixture is uniformly stirred, and then heating, keeping the temperature constant and cooling to obtain modified dimethyl silicone oil;
(3) mixing the modified dimethyl silicone oil, the modified polysiloxane, the emulsifier and the polypropylene glycol, stirring, adding the organic bentonite, and dispersing at a high speed to obtain the defoaming agent.
The surface tension of the dimethyl silicone oil is low, and the foam breaking is rapid; the hydrophobic white carbon black has small particle size and large enough specific surface area, can improve the dispersibility of the dimethyl silicone oil, enables the dimethyl silicone oil to form a large number of small defoaming units, is easy to adsorb on a bubble liquid film and generates large force, and enables bubbles to be broken under the action of low surface tension of the dimethyl silicone oil, thereby exerting a synergistic effect and improving the defoaming effect; hydroxyl contained on the polypropylene glycol provides hydrogen bonds for the organobentonite in the dimethyl silicone oil, so that the organobentonite forms a three-dimensional network structure in the dimethyl silicone oil, and the white carbon black is filled in the three-dimensional network structure, so that the agglomeration and sedimentation of the white carbon black are reduced; the modified dimethyl silicone oil is mixed with the modified polysiloxane for use, so that the defoaming effect of the defoaming agent is further improved.
Preferably, the mass ratio of the white carbon black, the modified polysiloxane and the organic bentonite is 0.1 (5-7) to 0.2-0.4.
The mass ratio of the white carbon black, the modified polysiloxane and the organic bentonite is controlled within the range, and the defoaming performance of the prepared defoaming agent is greatly improved.
Preferably, the emulsifier is a mixture of Span-80 and tween-80.
Preferably, the modified polysiloxane is prepared by the following steps:
(A) mixing low hydrogen-containing polysiloxane and concentrated sulfuric acid, stirring until the mixture is uniformly mixed, heating in an oil bath, adding trifluoropropylmethyl cyclotrisiloxane for reaction, neutralizing with sodium bicarbonate, removing residual water with anhydrous sodium sulfate, and removing unreacted micromolecules under a reduced pressure condition to obtain a mixture;
(B) mixing polyether and acetic anhydride, heating, reacting under the protection of nitrogen, vacuumizing after the reaction is finished, and then removing unreacted acetic anhydride by nitrogen purging to obtain acetyl-terminated allyl polyether;
(C) mixing acetyl terminated allyl polyether and toluene, adding chloroplatinic acid and sodium citrate, reacting under the protection of nitrogen, stirring and heating after the reaction is finished, and uniformly mixing; and (B) adding the mixture prepared in the step (A), heating for reaction, and removing the solvent from the product through rotary distillation after the reaction is finished to obtain the modified polysiloxane.
The low-hydrogen polysiloxane has lower surface tension, thereby having better defoaming capability; the trifluoropropyl methyl cyclotrisiloxane has higher surface activity, so that the trifluoropropyl methyl cyclotrisiloxane has higher defoaming capability, and the fluoroalkyl is grafted on the low-hydrogen polysiloxane, so that the stability of the modified polysiloxane is effectively improved; the acetyl-terminated allyl polyether is grafted to the low-hydrogen polysiloxane, so that the solubility of the modified polysiloxane is effectively improved, and the foam inhibition capability of the modified polysiloxane is improved.
Preferably, the mass ratio of the low hydrogen polysiloxane to the trifluoropropylmethylcyclotrisiloxane to the polyether is 2 (0.5-0.7) to (0.7-0.9).
The mass ratio of the low hydrogen-containing polysiloxane, the trifluoropropylmethyl cyclotrisiloxane and the polyether is controlled within the range, and the defoaming performance of the prepared defoaming agent is greatly improved.
Preferably, the rosin is one or more of water white hydrogenated rosin, hydrogenated rosin glyceride and KE-100 rosin.
Preferably, the surfactant is one or more of OP-10, Tween-80 and span-20.
Preferably, the soldering flux is prepared by the following steps:
heating and melting rosin until the rosin is completely melted; and then adding o-iodobenzoic acid, tetrahydrofurfuryl alcohol, a surfactant, triphenylphosphine oxide and a defoaming agent, keeping the temperature, continuously stirring until the o-iodobenzoic acid, the tetrahydrofurfuryl alcohol, the surfactant, the triphenylphosphine oxide and the defoaming agent are completely dissolved, and cooling to obtain the soldering flux.
Preferably, the preparation method of the high-performance tin soldering rod comprises the following steps: the method comprises the following steps:
s1, uniformly mixing tin and copper, pouring into a die, and cooling to obtain a hollow tin alloy;
and S2, pouring the soldering flux into the hollow tin alloy through an extrusion process to obtain the tin soldering rod.
In summary, the present application includes at least one of the following beneficial technical effects:
1. the o-iodobenzoic acid can remove oxides on the surfaces of the solder and the base material, so that the solder is contacted with the pure base material, and the wetting is effectively finished; the tetrahydrofurfuryl alcohol contributes to a polar environment provided during welding, so that H ions in the active agent are ionized to exert activity; the surface active agent can reduce the surface tension of the liquid soldering flux, so that the soldering flux can smoothly spread on the surface of the base material to remove an oxide film on the surface of the base material, and can reduce the surface tension of the solder and enhance the wetting capacity of the solder to the base material; the triphenylphosphine oxide can form a layer of film on the surface of the substrate so as to play a role in protection and improve the corrosivity remained after welding; the rosin has film forming property, can protect a welding part from being oxidized at high temperature in welding, and a hydrophobic protective film formed after welding has excellent electrical insulation property; the defoaming agent can reduce the splashing phenomenon in the welding process, thereby reducing the damage to workers.
2. The surface tension of the dimethyl silicone oil is low, and the bubbles can be broken quickly; the hydrophobic white carbon black has a large enough specific surface area, can improve the dispersibility of the dimethyl silicone oil, is very easy to adsorb on a bubble liquid film and generates a large force, and bubbles are broken under the action of low surface tension of the dimethyl silicone oil, so that a synergistic effect is exerted, and the defoaming effect is improved; hydroxyl contained on the polypropylene glycol provides hydrogen bonds for the organic bentonite in the dimethyl silicone oil, so that the agglomeration and sedimentation of the white carbon black are reduced; the modified dimethyl silicone oil is mixed with the modified polysiloxane for use, so that the defoaming effect of the defoaming agent is further improved.
3. The low hydrogen-containing polysiloxane has lower surface tension, thereby having better defoaming capability; the trifluoropropylmethylcyclotrisiloxane has higher surface activity, so that the trifluoropropylmethylcyclotrisiloxane has higher defoaming capability, and fluoroalkyl is grafted to low-hydrogen polysiloxane, so that the stability of the modified polysiloxane is effectively improved; the acetyl-terminated allyl polyether is grafted to the low-hydrogen polysiloxane, so that the solubility of the modified polysiloxane is effectively improved, and the foam inhibition capability of the modified polysiloxane is improved.
Detailed Description
The embodiment of the application discloses a high-performance soldering tin rod and a preparation method thereof.
Example 1
The modified polysiloxane comprises the following raw materials: 20g of low hydrogen polysiloxane, 5g of trifluoropropylmethyl cyclotrisiloxane and 9g of polyether.
The modified polysiloxane is prepared by the following steps:
(A) mixing low hydrogen-containing polysiloxane and 8g of concentrated sulfuric acid, stirring until the mixture is uniformly mixed, heating the mixture to 100 ℃ in an oil bath, adding trifluoropropylmethylcyclotrisiloxane, reacting for 2 hours, neutralizing with sodium bicarbonate, removing residual moisture with anhydrous sodium sulfate, and removing unreacted micromolecules under the reduced pressure environment of 0.01Mpa and 80 ℃ to obtain a mixture;
(B) mixing polyether and 1g of acetic anhydride, heating to 120 ℃, reacting for 3 hours under the protection of nitrogen, vacuumizing after the reaction is finished, and then removing unreacted acetic anhydride by nitrogen purging to obtain acetyl-terminated allyl polyether;
(C) mixing acetyl-terminated allyl polyether and 30g of toluene, adding 4g of chloroplatinic acid and 4g of sodium citrate, reacting for 10min under the protection of nitrogen, stirring and heating to 70 ℃ after the reaction is finished, and uniformly mixing; and (C) adding the mixture prepared in the step (A), heating to 110 ℃, reacting for 6 hours, and removing the solvent from the product after the reaction is finished by rotary distillation to obtain the modified polysiloxane.
The defoaming agent comprises the following raw materials: 1g of white carbon black, 50g of modified polysiloxane and 4g of organic bentonite.
The defoaming agent is prepared by the following steps:
(1) mixing 2g of octamethylcyclotetrasiloxane and white carbon black, adding 0.01g of NaOH, reacting at 100 ℃ for 4 hours, and cooling after the reaction is finished to prepare hydrophobic white carbon black;
(2) mixing 10g of dimethyl silicone oil and hydrophobic white carbon black, stirring until the mixture is uniformly stirred, heating to 190 ℃, keeping the temperature for 5 hours, cooling to 50 ℃, and modifying the dimethyl silicone oil;
(3) mixing modified dimethyl silicone oil, modified polysiloxane, 3g of emulsifier and 1g of polypropylene glycol, stirring for 20min at 110 ℃, adding organic bentonite, and dispersing at high speed of 14000rpm/min for 9min in a homogenizer to obtain the defoaming agent.
Wherein the emulsifier is a mixture of Span-80 and Tween-80.
The soldering flux comprises the following raw materials: 12g of o-iodobenzoic acid, 2g of tetrahydrofurfuryl alcohol, 0.6g of surfactant, 1g of triphenylphosphine oxide, 0.1g of defoaming agent and 86.3g of rosin.
The soldering flux is prepared by the following steps:
heating and melting rosin at 120 ℃ until the rosin is completely melted; and adding o-iodobenzoic acid, tetrahydrofurfuryl alcohol, a surfactant, triphenylphosphine oxide and a defoaming agent, keeping the temperature, continuously stirring until the o-iodobenzoic acid, the tetrahydrofurfuryl alcohol, the surfactant, the triphenylphosphine oxide and the defoaming agent are completely dissolved, and cooling to obtain the soldering flux.
Wherein the surfactant is a mixture of OP-10 and Tween-80, and the rosin is a mixture of water-white hydrogenated rosin and KE-100 rosin.
A preparation method of a high-performance solder tin rod comprises the following steps:
s1, uniformly mixing tin and copper, pouring into a die, and cooling to obtain a hollow tin alloy;
and S2, pouring the soldering flux into the hollow tin alloy through an extrusion process to obtain the tin soldering rod.
Example 2
The modified polysiloxane comprises the following raw materials: 20g of low hydrogen polysiloxane, 7g of trifluoropropylmethyl cyclotrisiloxane and 7g of polyether.
The modified polysiloxane is prepared by the following steps:
(A) mixing low hydrogen-containing polysiloxane and 8g of concentrated sulfuric acid, stirring until the mixture is uniformly mixed, heating in an oil bath to 110 ℃, adding trifluoropropyl methyl cyclotrisiloxane, reacting for 1h, neutralizing with sodium bicarbonate, removing residual moisture with anhydrous sodium sulfate, and removing unreacted micromolecules under the reduced pressure environment of 0.03MPa and 70 ℃ to obtain a mixture;
(B) mixing polyether and 1g of acetic anhydride, heating to 140 ℃, reacting for 2 hours under the protection of nitrogen, vacuumizing after the reaction is finished, and then removing unreacted acetic anhydride by nitrogen purging to obtain acetyl-terminated allyl polyether;
(C) mixing acetyl-terminated allyl polyether and 30g of toluene, adding 4g of chloroplatinic acid and 4g of sodium citrate, reacting for 12min under the protection of nitrogen, stirring after the reaction is finished, and heating to 60 ℃ to uniformly mix the allyl polyether and the toluene; and (C) adding the mixture prepared in the step (A), heating to 130 ℃, reacting for 5 hours, and removing the solvent from the product after the reaction is finished by rotary distillation to obtain the modified polysiloxane.
The defoaming agent comprises the following raw materials: 0.1g of white carbon black, 70g of modified polysiloxane and 2g of organic bentonite.
The defoaming agent is prepared by the following steps:
(1) mixing 2g of octamethylcyclotetrasiloxane and white carbon black, adding 0.01g of NaOH, reacting at 120 ℃ for 2 hours, and cooling after the reaction is finished to prepare hydrophobic white carbon black;
(2) mixing 10g of dimethyl silicone oil and hydrophobic white carbon black, stirring until the mixture is uniformly stirred, heating to 210 ℃, keeping the temperature for 3 hours, cooling to 60 ℃, and modifying the dimethyl silicone oil;
(3) mixing modified dimethyl silicone oil, modified polysiloxane, 3g of emulsifier and 1g of polypropylene glycol, stirring for 15min at 130 ℃, then adding organic bentonite, and dispersing for 5min at a high speed of 16000rpm/min in a homogenizer to obtain the defoaming agent.
Wherein the emulsifier is a mixture of Span-80 and Tween-80.
The soldering flux comprises the following raw materials: 16g of o-iodobenzoic acid, 6g of tetrahydrofurfuryl alcohol, 0.8g of surfactant, 3g of triphenylphosphine oxide, 0.5g of defoaming agent and 73.7g of rosin.
The soldering flux is prepared by the following steps:
heating and melting rosin at 140 ℃ until the rosin is completely melted; and adding o-iodobenzoic acid, tetrahydrofurfuryl alcohol, a surfactant, triphenylphosphine oxide and a defoaming agent, keeping the temperature, continuously stirring until the o-iodobenzoic acid, the tetrahydrofurfuryl alcohol, the surfactant, the triphenylphosphine oxide and the defoaming agent are completely dissolved, and cooling to obtain the soldering flux.
Wherein the surfactant Tween-80, and the rosin is water white hydrogenated rosin.
A preparation method of a high-performance solder tin rod comprises the following steps:
s1, uniformly mixing tin and copper, pouring into a die, and cooling to obtain a hollow tin alloy;
and S2, pouring the soldering flux into the hollow tin alloy through an extrusion process to obtain the tin soldering rod.
Example 3
The modified polysiloxane comprises the following raw materials: 20g of low hydrogen polysiloxane, 6g of trifluoropropylmethyl cyclotrisiloxane and 8g of polyether.
The modified polysiloxane is prepared by the following steps:
(A) mixing low hydrogen-containing polysiloxane and 8g of concentrated sulfuric acid, stirring until the mixture is uniformly mixed, heating the mixture to 105 ℃ in an oil bath, adding trifluoropropylmethylcyclotrisiloxane, reacting for 1.5h, neutralizing with sodium bicarbonate, removing residual moisture with anhydrous sodium sulfate, and removing unreacted micromolecules under the reduced pressure environment of 0.02Mpa and 75 ℃ to obtain a mixture;
(B) mixing polyether and 1g of acetic anhydride, heating to 130 ℃, reacting for 2.5 hours under the protection of nitrogen, vacuumizing after the reaction is finished, and then blowing nitrogen to remove unreacted acetic anhydride to obtain acetyl-terminated allyl polyether;
(C) mixing acetyl-terminated allyl polyether and 30g of toluene, adding 4g of chloroplatinic acid and 4g of sodium citrate, reacting for 11min under the protection of nitrogen, stirring after the reaction is finished, and heating to 65 ℃ to uniformly mix the allyl polyether and the toluene; and (C) adding the mixture prepared in the step (A), heating to 120 ℃, reacting for 5.5 hours, and removing the solvent from the product after the reaction is finished by rotary distillation to obtain the modified polysiloxane.
The defoaming agent comprises the following raw materials: 1g of white carbon black, 60g of modified polysiloxane and 3g of organic bentonite.
The defoaming agent is prepared by the following steps:
(1) mixing 2g of octamethylcyclotetrasiloxane and white carbon black, adding 0.01g of NaOH, reacting at 110 ℃ for 3 hours, and cooling after the reaction is finished to prepare hydrophobic white carbon black;
(2) mixing 10g of dimethyl silicone oil and hydrophobic white carbon black, stirring until the mixture is uniformly stirred, heating to 200 ℃, keeping the temperature for 4 hours, cooling to 55 ℃, and modifying the dimethyl silicone oil;
(3) mixing modified dimethyl silicone oil, modified polysiloxane, 3g of emulsifier and 1g of polypropylene glycol, stirring for 18min at 120 ℃, adding organic bentonite, and dispersing for 7min at a high speed of 15000rpm/min in a homogenizer to obtain the defoaming agent.
Wherein the emulsifier is a mixture of Span-80 and Tween-80.
The soldering flux comprises the following raw materials: 14g of o-iodobenzoic acid, 4g of tetrahydrofurfuryl alcohol, 0.7g of surfactant, 2g of triphenylphosphine oxide, 0.3g of defoaming agent and 79g of rosin.
The soldering flux is prepared by the following steps:
heating and melting rosin at 130 ℃ until the rosin is completely melted; and adding o-iodobenzoic acid, tetrahydrofurfuryl alcohol, a surfactant, triphenylphosphine oxide and a defoaming agent, keeping the temperature, continuously stirring until the o-iodobenzoic acid, the tetrahydrofurfuryl alcohol, the surfactant, the triphenylphosphine oxide and the defoaming agent are completely dissolved, and cooling to obtain the soldering flux.
Wherein the surfactant span-20 and the rosin is hydrogenated rosin glyceride.
A preparation method of a high-performance solder tin rod comprises the following steps:
s1, uniformly mixing tin and copper, pouring into a die, and cooling to obtain a hollow tin alloy;
and S2, pouring the soldering flux into the hollow tin alloy through an extrusion process to obtain the tin soldering rod.
Example 4
Example 4 differs from example 3 in that: 1.9g of white carbon black, 56.5g of modified polysiloxane and 5.6g of organic bentonite.
Example 5
Example 5 differs from example 3 in that: 0.7g of white carbon black, 61.3g of modified polysiloxane and 2g of organic bentonite.
Example 6
Example 6 differs from example 3 in that: 1g of white carbon black, 62g of modified polysiloxane and 1g of organic bentonite.
Example 7
Example 7 differs from example 3 in that: 1g of white carbon black, 58g of modified polysiloxane and 5g of organic bentonite.
Example 8
Example 8 differs from example 3 in that: 22g of low hydrogen polysiloxane, 3g of trifluoropropylmethyl cyclotrisiloxane and 9g of polyether.
Example 9
Example 9 differs from example 3 in that: 19g of low hydrogen polysiloxane, 8g of trifluoropropylmethyl cyclotrisiloxane and 7g of polyether.
Example 10
Example 10 differs from example 3 in that: 22g of low hydrogen polysiloxane, 7g of trifluoropropylmethyl cyclotrisiloxane and 5g of polyether.
Example 11
Example 11 differs from example 3 in that: 18g of low hydrogen polysiloxane, 6g of trifluoropropylmethyl cyclotrisiloxane and 10g of polyether.
Comparative example 1
Comparative example 1 differs from example 3 in that: 16g of white carbon black, 0g of modified polysiloxane and 48 g of organic bentonite.
Comparative example 2
Comparative example 2 differs from example 3 in that: 1g of white carbon black, 63g of modified polysiloxane and 0g of organic bentonite.
Comparative example 3
Comparative example 3 differs from example 3 in that: 24g of low hydrogen polysiloxane, 0g of trifluoropropylmethyl cyclotrisiloxane and 10g of polyether.
Comparative example 4
Comparative example 4 differs from example 3 in that: 26g of low hydrogen polysiloxane, 8g of trifluoropropylmethyl cyclotrisiloxane and 0g of polyether.
The solder rods prepared in examples 1 to 11 and comparative examples 1 to 4 were sampled and the samples were subjected to a property test.
Splash-proof performance detection
(1) The spatter rate was measured by the International Association for electronic industries red method, and the lower the spatter rate, the better the spatter resistance of the solder bar, and the test results are reported in Table 1.
F S ＝(X 2 -X 1 )/(W 1 -W 2 )*F
F S The spattering rate (%) of the flux; x 2 Weight (g) of aluminum foil plus spatter; x 1 Weight (g) of aluminum foil; w 1 Weight (g) of the solder bar before soldering; w 2 Weight (g) of the post-soldering tin rod; f is the proportion (%) of the soldering flux in the soldering aid rod.
(2) The samples were visually observed for spatter during welding and the results are reported in table 1.
TABLE 1
Data analysis
As can be seen from Table 1, the amount of spatter of the solder rods in examples 1 to 3 was 8.5 to 10.2%, and there was substantially no spatter observed with naked eyes, so that it can be seen that the solder rods prepared by the present invention had good spatter prevention performance.
As can be seen from table 1, example 4 differs from example 3 in that: 1g of white carbon black, 60g of modified polysiloxane and 3g of organic bentonite in example 3, 1.9g of white carbon black, 56.5g of modified polysiloxane and 5.6g of organic bentonite in example 4, wherein the splash amount in example 3 is 8.5%, the splash is almost not splashed when observed by naked eyes, the splash amount in example 4 is 17.7%, a small amount of splash exists when observed by naked eyes, and the splash preventing effect is obviously reduced in example 4 compared with example 3; this is because when the content of the modified polysiloxane is reduced, on the one hand, the defoaming ability of the modified polysiloxane is reduced, and on the other hand, the synergistic effect of the modified dimethylsilicone oil and the modified polysiloxane is reduced, thereby reducing the spattering preventing performance of the solder bar.
As can be seen from table 1, example 5 differs from example 3 in that: 1g of white carbon black, 60g of modified polysiloxane and 3g of organic bentonite in example 3, 0.7g of white carbon black in example 5, 61.3g of modified polysiloxane and 2g of organic bentonite, wherein the splashing amount in example 3 is 8.5%, almost no splashing is observed by naked eyes, the splashing amount in example 5 is 18.3%, a small amount of splashing is observed by naked eyes, and the anti-splashing effect is obviously reduced compared with that in example 3 in example 5; this is because when the content of the modified polysiloxane is increased, the content of the white carbon black and the content of the organobentonite are reduced, on one hand, the dispersibility of the dimethicone is reduced, the defoaming capability of the dimethicone is weakened, and the synergistic effect of the modified dimethicone and the modified polysiloxane is weakened; on the other hand, the white carbon black is easy to agglomerate, so that the synergistic action of the white carbon black and the dimethyl silicone oil is weakened, and the anti-splashing performance of the tin welding rod is reduced.
As can be seen from table 1, example 6 differs from example 3 in that: 1g of white carbon black, 60g of modified polysiloxane and 3g of organic bentonite in example 3, 1g of white carbon black, 62g of modified polysiloxane and 1g of organic bentonite in example 6, wherein the splashing amount in example 3 is 8.5%, the splashing is almost not generated by visual observation, the splashing amount in example 6 is 17.2%, a small amount of splashing exists by visual observation, and the splashing prevention effect is obviously reduced compared with that in example 3 in example 6; this is because when the content of the organobentonite is reduced, the white carbon black is likely to agglomerate, so that the synergistic effect of the white carbon black and the dimethyl silicone oil is weakened, and the anti-splashing performance of the solder rod is reduced.
As can be seen from table 1, example 7 differs from example 3 in that: in example 3, 1g of white carbon black, 60g of modified polysiloxane and 3g of organic bentonite, in example 7, 1g of white carbon black, 58g of modified polysiloxane, 5g of organic bentonite, and in example 3, the amount of splashes is 8.5%, almost no splashes are observed by naked eyes, in example 7, the amount of splashes is 18.1%, and a small amount of splashes are observed by naked eyes, so that compared with example 3, the splash prevention effect is obviously reduced, because when the content of the organic bentonite is increased, the content of the modified polysiloxane is reduced, on one hand, the foam inhibition capability of the poly-modified polysiloxane is reduced, and on the other hand, the synergistic effect of the modified dimethyl silicone oil and the modified polysiloxane is weakened, so that the splash prevention performance of the tin welding rod is reduced.
As can be seen from table 1, example 8 differs from example 3 in that: 20g of low hydrogenpolysiloxane in example 3, 6g of trifluoropropylmethylcyclotrisiloxane and 8g of polyether, 22g of low hydrogenpolysiloxane in example 8, 3g of trifluoropropylmethylcyclotrisiloxane and 9g of polyether, wherein the splashing amount in example 3 is 8.5%, almost no splashing is observed by naked eyes, the splashing amount in example 8 is 13.5%, slight splashing exists by naked eyes, and the splashing prevention effect in example 8 is obviously reduced compared with that in example 3; this is because when the content of trifluoropropylmethylcyclotrisiloxane is reduced, the amount of fluoroalkyl groups grafted to the low hydrogen-containing polysiloxane is reduced, the stability of the modified polysiloxane is reduced, the synergistic effect of the modified polysiloxane and the modified dimethylsilicone oil is weakened, and the spattering prevention performance of the solder bar is reduced.
As can be seen from table 1, example 9 differs from example 3 in that: 20g of low-hydrogen polysiloxane in example 3, 6g of trifluoropropylmethylcyclotrisiloxane and 8g of polyether, 19g of low-hydrogen polysiloxane in example 9, 8g of trifluoropropylmethylcyclotrisiloxane and 7g of polyether, wherein the spattering amount in example 3 is 8.5%, spattering hardly occurs by visual observation, the spattering amount in example 9 is 12.9%, slight spattering exists by visual observation, and the spattering prevention effect in example 9 is remarkably reduced as compared with example 3; this is because when the content of trifluoropropylmethylcyclotrisiloxane is increased, the content of low hydrogen-containing polysiloxane is decreased, thereby decreasing the defoaming ability of modified polysiloxane, so that the synergistic effect of modified polysiloxane and modified dimethylsilicone oil is weakened, and the anti-spattering property of the solder bar is decreased.
As can be seen from table 1, example 10 differs from example 3 in that: 20g of low hydrogenpolysiloxane in example 3, 6g of trifluoropropylmethylcyclotrisiloxane and 8g of polyether, 22g of low hydrogenpolysiloxane in example 10, 7g of trifluoropropylmethylcyclotrisiloxane and 5g of polyether, wherein the splashing amount in example 3 is 8.5%, almost no splashing is observed by naked eyes, the splashing amount in example 10 is 13.1%, slight splashing exists by naked eyes, and the splashing prevention effect in example 10 is obviously reduced compared with that in example 3; this is because, when the content of polyether is reduced, acetyl group-terminated allyl polyether grafted to low hydrogen-containing polysiloxane is reduced, the foam suppressing ability of modified polysiloxane is reduced, the synergistic effect of modified polysiloxane and dimethylsilicone oil is weakened, and the spatter preventing property of the solder bar is reduced.
As can be seen from table 1, example 11 differs from example 3 in that: 20g of low-hydrogen polysiloxane in example 3, 6g of trifluoropropylmethylcyclotrisiloxane and 8g of polyether in example 11, 18g of low-hydrogen polysiloxane in example 11, 6g of trifluoropropylmethylcyclotrisiloxane and 10g of polyether in example 3, and the amount of spatter in example 3 was 8.5%, and almost no spatter was observed with naked eyes, and the amount of spatter in example 11 was 12.8%, and slight spatter was observed with naked eyes, and the spatter-preventing effect was remarkably reduced in example 11 as compared with example 3; this is because when the content of the polyether is increased, the content of the low hydrogen-containing polysiloxane is decreased, thereby decreasing the defoaming ability of the modified polysiloxane, so that the synergistic effect of the modified polysiloxane and the modified dimethylsilicone oil is weakened, thereby decreasing the spatter preventing performance of the solder bar.
As can be seen from table 1, comparative example 1 and example 3 differ in that: 1g of white carbon black, 60g of modified polysiloxane and 3g of organic bentonite in example 3, 16g of white carbon black, 0g of modified polysiloxane and 48 g of organic bentonite in comparative example 1, wherein the splashing amount in example 3 is 8.5%, the splashing is almost not generated by visual observation, the splashing amount in comparative example 1 is 78.2%, the severe splashing exists by visual observation, and the anti-splashing effect is obviously reduced compared with that in comparative example 1 and example 3; this is because, when the defoaming agent does not contain the modified polysiloxane, the spatter preventing performance of the solder bar is lowered.
As can be seen from table 1, comparative example 2 and example 3 differ in that: 1g of white carbon black, 60g of modified polysiloxane and 3g of organic bentonite in example 3, 1g of white carbon black, 63g of modified polysiloxane and 0g of organic bentonite in comparative example 2, wherein the splashing amount in example 3 is 8.5%, the splashing is almost not generated by visual observation, the splashing amount in comparative example 2 is 32.5%, more splashing exists by visual observation, and the splashing prevention effect is obviously reduced compared with that in comparative example 2 and example 3; the reason is that when the defoaming agent does not contain organic bentonite, the white carbon black is easy to agglomerate, so that the synergistic action of the white carbon black and the dimethyl silicone oil is reduced, and the synergistic action of the modified dimethyl silicone oil and the modified polysiloxane is weakened, so that the anti-splashing performance of the tin rod is reduced.
As can be seen from table 1, comparative example 3 and example 3 differ in that: 20g of low hydrogen polysiloxane in example 3, 6g of trifluoropropylmethylcyclotrisiloxane and 8g of polyether, 24g of low hydrogen polysiloxane in comparative example 3, 0g of trifluoropropylmethylcyclotrisiloxane and 10g of polyether, wherein the splashing amount in example 3 is 8.5%, almost no splashing is observed by naked eyes, the splashing amount in comparative example 3 is 27.5%, more splashing is observed by naked eyes, and the splashing prevention effect is obviously reduced compared with that in comparative example 3 and example 3; the reason is that when the modified polysiloxane does not contain trifluoropropylmethylcyclotrisiloxane in the preparation process, the modified polysiloxane is poor in stability, the defoaming capability of the modified polysiloxane is reduced, and the synergistic effect of the modified polysiloxane and the modified dimethylsilicone oil is reduced, so that the anti-splashing performance of the tin welding rod is reduced.
As can be seen from table 1, comparative example 4 differs from example 3 in that: 20g of low hydrogen polysiloxane in example 3, 6g of trifluoropropylmethylcyclotrisiloxane and 8g of polyether, 18g of low hydrogen polysiloxane in comparative example 4, 6g of trifluoropropylmethylcyclotrisiloxane and 10g of polyether, wherein the splashing amount in example 3 is 8.5%, almost no splashing is observed by naked eyes, the splashing amount in comparative example 4 is 29.2%, more splashing is observed by naked eyes, and the splashing prevention effect is obviously reduced compared with that in comparative example 4 and example 3; the reason is that when the modified polysiloxane does not contain polyether in the preparation process, the solubility of the modified polysiloxane is poor, and the foam inhibition capability of the modified polysiloxane is reduced, so that the synergistic effect of the modified polysiloxane and the modified dimethyl silicone oil is reduced, and the anti-splashing performance of the tin welding rod is reduced.
The present embodiment is merely illustrative and not restrictive, and various changes and modifications may be made by persons skilled in the art without departing from the scope of the present invention as defined in the appended claims. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. A high-performance solder tin rod is characterized in that: the soldering flux comprises a hollow tin alloy and a soldering flux filled in the tin alloy, wherein the soldering flux comprises the following raw materials in percentage by mass: 10-12% of o-iodobenzoic acid, 2-4% of tetrahydrofurfuryl alcohol, 0.6-0.8% of surfactant, 1-2% of triphenylphosphine oxide, 0.1-0.2% of defoaming agent and the balance of rosin.
2. The high performance solder stick of claim 1, wherein: the defoaming agent is prepared by the following steps:
(1) mixing octamethylcyclotetrasiloxane and white carbon black, adding NaOH for heating reaction, and cooling after the reaction is finished to prepare hydrophobic white carbon black;
(2) mixing the dimethyl silicone oil and the hydrophobic white carbon black, stirring until the mixture is uniformly stirred, and then heating, keeping the temperature constant and cooling to obtain modified dimethyl silicone oil;
(3) mixing the modified dimethyl silicone oil, the modified polysiloxane, the emulsifier and the polypropylene glycol, stirring, adding the organic bentonite, and dispersing at a high speed to obtain the defoaming agent.
3. The high performance solder bar of claim 2, wherein: the mass ratio of the white carbon black, the modified polysiloxane and the organic bentonite is 0.1 (5-7) to 0.2-0.4.
4. The high performance solder stick of claim 2, wherein: the emulsifier is a mixture of Span-80 and Tween-80.
5. The high performance solder stick of claim 2, wherein: the modified polysiloxane is prepared by the following steps:
(A) mixing low hydrogen-containing polysiloxane and concentrated sulfuric acid, stirring until the mixture is uniformly mixed, heating in an oil bath, adding trifluoropropylmethyl cyclotrisiloxane for reaction, neutralizing with sodium bicarbonate, removing residual water with anhydrous sodium sulfate, and removing unreacted micromolecules under a reduced pressure condition to obtain a mixture;
(B) mixing polyether and acetic anhydride, heating, reacting under the protection of nitrogen, vacuumizing after the reaction is finished, and removing unreacted acetic anhydride by using nitrogen purging to obtain acetyl-terminated allyl polyether;
(C) mixing acetyl terminated allyl polyether and toluene, adding chloroplatinic acid and sodium citrate, reacting under the protection of nitrogen, stirring and heating after the reaction is finished, and uniformly mixing; and (B) adding the mixture prepared in the step (A), heating for reaction, and after the reaction is finished, carrying out rotary distillation on the product to remove the solvent, thereby obtaining the modified polysiloxane.
6. The high performance solder stick of claim 5, wherein: the mass ratio of the low hydrogen polysiloxane, the trifluoropropylmethylcyclotrisiloxane to the polyether is 2 (0.5-0.7) to 0.7-0.9.
7. The high performance solder stick of claim 1, wherein: the rosin is one or more of water white hydrogenated rosin, hydrogenated rosin glyceride and KE-100 rosin.
8. The high performance solder stick of claim 1, wherein: the surfactant is one or more of OP-10, Tween-80 and span-20.
9. The high performance solder bar of claim 1, in which: the soldering flux is prepared by the following steps:
heating and melting rosin until the rosin is completely melted; and adding o-iodobenzoic acid, tetrahydrofurfuryl alcohol, a surfactant, triphenylphosphine oxide and a defoaming agent, keeping the temperature, continuously stirring until the o-iodobenzoic acid, the tetrahydrofurfuryl alcohol, the surfactant, the triphenylphosphine oxide and the defoaming agent are completely dissolved, and cooling to obtain the soldering flux.
10. A preparation method of a high-performance solder tin rod comprises the following steps: the method is characterized in that: the method comprises the following steps:
s1, uniformly mixing tin and copper, pouring into a die, and cooling to obtain a hollow tin alloy;
and S2, pouring the soldering flux into the hollow tin alloy through an extrusion process to obtain the tin soldering rod.
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| CN115971719A (en) * | 2023-02-27 | 2023-04-18 | 深圳市唯特偶新材料股份有限公司 | Solder paste for improving welding cavity of large-area bonding pad of electronic device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115971719A (en) * | 2023-02-27 | 2023-04-18 | 深圳市唯特偶新材料股份有限公司 | Solder paste for improving welding cavity of large-area bonding pad of electronic device |
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