CN114749828A - Soldering flux for wave soldering and manufacturing method thereof - Google Patents
Soldering flux for wave soldering and manufacturing method thereof Download PDFInfo
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- CN114749828A CN114749828A CN202210518048.6A CN202210518048A CN114749828A CN 114749828 A CN114749828 A CN 114749828A CN 202210518048 A CN202210518048 A CN 202210518048A CN 114749828 A CN114749828 A CN 114749828A
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- flux
- soldering
- organic acid
- surfactant
- forming agent
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Classifications
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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
- B23K35/3612—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 with organic compounds as principal constituents
-
- 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
- B23K1/00—Soldering, e.g. brazing, or unsoldering
- B23K1/08—Soldering by means of dipping in molten solder
- B23K1/085—Wave soldering
-
- 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
-
- 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
Abstract
The application relates to a soldering flux for wave soldering and a manufacturing method thereof, wherein the soldering flux comprises the following raw materials in percentage by mass: 2-5% of an organic acid activator; 1.5 to 3.5 percent of surfactant; 0.5-1% of film-forming agent; 0.05 to 0.07 percent of corrosion inhibitor; the balance of carrier solvent; wherein the organic acid activator is a mixture of two or more of succinic acid, adipic acid, malic acid and sebacic acid; the surfactant is mixture of two or more of triethanolamine, butyl acetate, EDTA disodium and N-dodecyl alanine; the film forming agent is prepared from polyacrylamide, ethylene diamine tetramethylene sodium phosphate and polyethylene oxide according to the mass ratio of (1-1.2): (0.5-0.7): (0.2-0.4) mixing; the carrier solvent is prepared by mixing ethyl cellulose and an alcohol ether solvent according to the mass ratio of 1: 6. The flux soldering assisting device has the effects of improving the flux soldering effect and reducing the corrosion residue of the flux soldering.
Description
Technical Field
The application relates to the field of soldering flux, in particular to soldering flux for wave soldering and a manufacturing method thereof.
Background
At present, wave soldering technology is often adopted in the electronic industry in the process of soldering. Wave soldering is the soldering purpose which is achieved by directly contacting the soldering surface of the plug-in board with high-temperature liquid tin, the high-temperature liquid tin keeps an inclined surface, and the liquid tin forms a wave-like phenomenon by a special device, so the wave soldering is called as wave soldering.
The surface of a welded metal workpiece has dirt such as oxide, dust and the like to hinder the combination between the base metal of the workpiece and a welding flux, so that the welding flux is usually added in the welding process, and the welding flux comprises components such as an activating agent, a solvent, a surfactant, a film forming agent and the like; the activator in the flux removes the oxide on the surface of the metal matrix, the film-forming agent helps to reduce the oxidation of the metal surface, the oxide-free state of the surfaces is kept, the film-forming agent is combined with the oxide on the surface of the metal to be welded by the chemical action of the flux, and a liquid-state substance is formed at the welding temperature, so that the metal atoms on the surface of the metal part to be welded and the molten solder are mutually diffused, and the purpose of soldering connection is achieved. The quality of the wave soldering flux directly determines the reliability of subsequent products.
However, in the use process of the wave soldering flux, the water-soluble flux and the rosin flux have better solderability, but the residual corrosion is increased, which is not beneficial to the subsequent use of electronic products; the low-solid-content cleaning-free fluxing has less residual corrosion, but the fluxing effect is not as good as that of the water-soluble fluxing agent and the rosin fluxing agent.
In view of the above-mentioned related technical problems, the inventors consider that exploring a soldering flux with good soldering assisting effect and less residual corrosivity can help to further improve the application and economic value of the wave soldering flux.
Disclosure of Invention
In order to improve the soldering effect of the soldering flux and reduce the corrosion residue of the soldering flux, the application provides the soldering flux for wave soldering and the manufacturing method thereof.
In a first aspect, the flux for wave soldering provided by the application adopts the following technical scheme:
the soldering flux for wave soldering comprises the following raw materials in percentage by mass:
2-5% of an organic acid activator; 1.5 to 3.5 percent of surfactant; 0.5-1% of film-forming agent; 0.05 to 0.07 percent of corrosion inhibitor; the balance of carrier solvent;
wherein the organic acid activator is a mixture of two or more of succinic acid, adipic acid, malic acid and sebacic acid; the surfactant is a mixture of two or more of triethanolamine, butyl acetate, EDTA disodium and N-dodecyl alanine; the film forming agent is prepared from polyacrylamide, ethylene diamine tetramethylene sodium phosphate and polyethylene oxide according to the mass ratio of (1-1.2): (0.5-0.7): (0.2-0.4) mixing; the carrier solvent is prepared by mixing ethyl cellulose and an alcohol ether solvent according to the mass ratio of 1: 6.
By adopting the technical scheme, the carrier solvent prepared by mixing ethyl cellulose and an alcohol ether solvent according to the mass ratio of 1:6 can dissolve the components contained in the flux to serve as a carrier of each component, so that the flux becomes a uniform viscous liquid and has good structural stability and tinning property. The organic acid activator can remove the oxide on the surface of the welding pad and the welding flux at the welding temperature; the surface active agent can reduce the surface tension of the welding flux and increase the wettability of the welding flux to welding powder and a welding disc; the film forming agent is prepared from polyacrylamide, ethylene diamine tetramethylene sodium phosphate and polyethylene oxide according to the mass ratio of (1-1.2): (0.5-0.7): (0.2-0.4), the film-forming agent prepared by the method plays a role of a protective film at normal temperature, does not show activity, shows activity at a welding temperature, and can prevent reoxidation of a matrix by the formed protective layer.
According to the application, the organic acid activator, the surfactant and the film-forming agent are compounded according to a certain proportion and act together under a specific proportion, and the good film-forming barrier property of the film-forming agent can fully wrap and block the organic acid activator, so that the direct contact between the organic acid activator and the metal surface is reduced at normal temperature, the corrosivity of the organic acid activator is reduced, and the activation stability of the organic acid activator is ensured; after the welding temperature is reached, the film forming agent shows activity, the wrapping and blocking effects on the organic acid disappear, the organic acid activator is in full contact with the surface of the metal to be welded under the assistance of the surfactant with stronger wetting capacity, the oxide layer on the surface of the metal to be welded is decomposed efficiently and quickly, and the strong fluxing property is shown; the film forming agent after welding quickly solidifies and hardens residues after pyrolysis and prevents the continuous activation of the activator, thereby reducing the corrosivity of the flux residues.
A soldering flux solution system formed by compounding the components in the soldering flux according to a specific ratio has better viscosity and expansibility, so that the splashing condition is good during wave soldering, and the formation of tin beads is reduced; the good viscosity and expansibility can not block a soldering flux spray head of wave soldering, and is beneficial to the expansion of solder, so that welding spots are smooth and mellow, the surface of the soldered tin is clean and tidy, residues are less, and the subsequent long-term use of electronic equipment is not influenced.
Preferably, the mass ratio of the organic acid activator, the surfactant and the film forming agent is (3-4): 2: (0.6-0.7).
By adopting the technical scheme, the proportion ranges of the organic acid activator, the surfactant and the film forming agent are further limited, so that the combination and compounding of the three are more accurate, and the three can generate more outstanding synergistic cooperation under proper combination and compounding, and the problems of strong corrosivity and low oxidation resistance caused by more organic acid activators and less surfactants and reduced fluxing effect caused by more film forming agents and less surfactants can be avoided under the combination and compounding of the proportion; the good proportion of the three components can better promote the expansion and blocking effects of the film forming agent on the organic acid activator, form an anti-oxidation layer on the welding surface, promote the reaction activity of the organic acid activator and the spreadability of the solder at the welding temperature, further ensure that the soldering flux has better fluxing property and less corrosion residue, and also ensure that the soldering flux has stronger physical stability and oxidation resistance.
Preferably, the organic acid activator is prepared by mixing succinic acid, malic acid and sebacic acid according to the mass ratio of (1.7-1.9) to (1.5-1.7) to (1.2-1.4).
By adopting the technical scheme, the organic acid activator removes the pad and the oxide film of the solder in the form of metal soap by utilizing the carboxyl of the organic acid and metal ions. The organic acid activator prepared by mixing succinic acid, malic acid and sebacic acid according to the mass ratio of (1.7-1.9) to (1.5-1.7) to (1.2-1.4) has a wide boiling point and decomposition temperature, so that the organic acid activator can be better applied to wave soldering processing technologies at different temperatures; the three acids are combined and compounded according to a certain proportion range, the three acids are well compatible, and the three acids have high reaction activity under the combined action, so that the soldering flux is further promoted in the soldering assisting effect.
Preferably, the surfactant is prepared from triethanolamine, butyl acetate and N-dodecyl alanine according to the mass ratio of (1.5-1.7) to (1-1.5): (0.7-0.9) mixing.
By adopting the technical scheme, the addition of the surfactant is beneficial to improving the fluidity and wettability of the flux, reducing the surface tension of the flux and guiding the solder to diffuse to the periphery, so that a smooth welding spot is formed and the spreading is facilitated. In the application, triethanolamine, butyl acetate and N-dodecyl alanine are adopted according to the mass ratio of (1.5-1.7) to (1-1.5): (0.7-0.9) the surfactant prepared by mixing the components can generate neutralization reaction after being mixed with an organic acid activator to generate a neutralization product, and the neutralization product is unstable and can be rapidly decomposed at the welding temperature to regenerate organic acid and organic amine, so that the reactivity of the organic acid during welding is ensured; after the welding is finished, the residual organic acid is neutralized by the organic amine in the surfactant, so that the acidity of the residue is reduced, and the corrosion is reduced. The surfactant formed by mixing triethanolamine, butyl acetate and N-dodecyl alanine is good in compatibility with other components of the soldering flux, has certain complexation, can play a role of a stabilizer by matching with a film forming agent and a carrier solvent, realizes invisible dragging of other components in a soldering flux system, further promotes the structural stability of the soldering flux system, ensures the uniformity of liquid under the condition of no stress of the soldering flux, and reduces layering.
Preferably, the alcohol ether solvent is dipropylene glycol methyl ether, dipropylene glycol ethyl ether and butyl ether according to a mass ratio of 6: 3: 1, mixing to obtain the product.
By adopting the technical scheme, the composite material is prepared from dipropylene glycol methyl ether, dipropylene glycol ethyl ether and butyl ether according to the mass ratio of 6: 3: 1, the alcohol ether solvent prepared by mixing can be well mixed with ethyl cellulose to form a carrier solvent with good stability, and the carrier solvent can promote the dissolution and blending of other components in the soldering flux; the dipropylene glycol methyl ether, the dipropylene glycol ethyl ether and the butyl ether act together, so that the alcohol ether solvent has good protection and proper viscosity, the thermal decomposition temperature of the soldering flux can be increased, the viscosity and expansibility of the soldering flux can be adjusted, and the expansion rate is increased.
Preferably, the corrosion inhibitor is benzotriazole.
By adopting the technical scheme, the benzotriazole is added to inhibit the corrosion of the organic acid activator in the soldering flux to the metal to be soldered, so that the corrosivity of the soldering flux is reduced.
Preferably, the material also comprises the following raw materials in percentage by mass: 0.1-0.3% of antioxidant, wherein the antioxidant is one or more of 2, 6-di-tert-butyl-p-cresol, hydroquinone and catechol.
By adopting the technical scheme, the addition of the antioxidant can act with the film forming agent to further prevent oxidation, so that a film can be formed quickly after welding, the welding metal surface is protected in a blocking way, the oxidation resistance of the electronic element is improved, and the practical application effect of the soldering flux is also improved.
In a second aspect, the present application provides a method for manufacturing a flux for wave soldering, which adopts the following technical scheme: a manufacturing method of soldering flux for wave soldering comprises the following steps:
step 1, mixing ethyl cellulose and an alcohol ether solvent according to a mass ratio of 1:6, mixing, stirring at 60-70 ℃ until the mixture is completely and uniformly dissolved to form a non-rosin carrier solvent;
step 2, adding a surfactant into a carrier solvent, uniformly mixing, adding a film-forming agent and a corrosion inhibitor, and uniformly mixing to obtain a mixed solution;
and 3, heating the mixed solution to 100-145 ℃, adding an organic acid activator, and uniformly stirring to obtain the wave soldering flux.
By adopting the technical scheme, firstly, the ethyl cellulose and the alcohol ether solvent are mixed according to the mass ratio of 1:6, mixing to prepare a non-rosin carrier solvent to provide a matrix carrier for the soldering flux; and then adding other components according to the sequence of firstly adding the surfactant, secondly adding the film forming agent and other auxiliary agents, uniformly dispersing the firstly added surfactant in the carrier solution, and then adding the film forming agent, wherein the film forming agent has a barrier effect on the surfactant, so that the organic acid active agent and the surfactant which are added subsequently are conveniently blocked, and the organic acid active agent and the surfactant are prevented from reacting to reduce the activity of the activator.
In summary, the present application includes at least one of the following beneficial technical effects:
1. according to the application, the organic acid activator, the surfactant and the film-forming agent are compounded according to a certain proportion and act together under a specific proportion, and the good film-forming barrier property of the film-forming agent can fully wrap and block the organic acid activator, so that the direct contact between the organic acid activator and the metal surface is reduced at normal temperature, the corrosivity of the organic acid activator is reduced, and the activation stability of the organic acid activator is ensured; after the welding temperature is reached, the film forming agent shows activity, the wrapping and blocking effects on the organic acid disappear, the organic acid activator is in full contact with the surface of the metal to be welded under the assistance of the surfactant with stronger wetting capacity, the oxide layer on the surface of the metal to be welded is decomposed efficiently and quickly, and the strong fluxing property is shown; the film forming agent after welding quickly solidifies, hardens and prevents the activating agent from continuously activating the residues after high-temperature decomposition, thereby reducing the corrosivity of the flux residues;
2. in the application, the surfactant is prepared by mixing triethanolamine, butyl acetate and N-dodecyl alanine according to a certain proportion, and the surfactant can ensure the reaction activity during the welding of organic acid; after the welding is finished, the residual organic acid can be neutralized by organic amine in the surfactant, so that the acidity of the residue is reduced, and the corrosion is reduced; the surfactant formed by mixing triethanolamine, butyl acetate and N-dodecyl alanine is good in compatibility with other components of the soldering flux and has certain complexation, and the surfactant can play a role of a stabilizer by matching with a film forming agent and a carrier solvent, so that the other components in a soldering flux system are invisibly dragged, the structural stability of the soldering flux system is further promoted, the uniformity of liquid can be guaranteed under the condition that the soldering flux is not stressed, and the layering is reduced;
3. the soldering flux solution system formed by compounding the components in the soldering flux according to the specific proportion has better viscosity and expansibility, so that the splashing condition is good during wave soldering, and the formation of tin beads is reduced; the good viscosity and expansibility can not block a soldering flux spray head of wave soldering, and is beneficial to the expansion of solder, so that welding spots are smooth and mellow, the surface of the soldered board is clean and tidy, residues are less, and the subsequent long-term use of electronic elements is not influenced.
Detailed Description
The present application will be described in further detail below with reference to preparation examples, and comparative examples.
Preparation example
Preparation example 1
The preparation example discloses a preparation method of an organic acid activator, which specifically comprises the following steps:
adding 5g of succinic acid and 5g of adipic acid into a stirrer, and stirring for 5min at the normal temperature and the rotation speed of 70r/min to obtain the organic acid activator.
Preparation example 2
The preparation example discloses a preparation method of an organic acid activator, which specifically comprises the following steps:
adding 3g of adipic acid, 4g of malic acid and 3g of sebacic acid into a stirrer, and stirring for 7min at the normal temperature and the rotation speed of 70r/min to obtain the organic acid activator.
Preparation example 3
The preparation example discloses a preparation method of an organic acid activator, which specifically comprises the following steps:
adding 2.5g of succinic acid, 2.5g of adipic acid, 2.5g of malic acid and 2.5g of sebacic acid into a stirrer, and stirring for 10min at the normal temperature and the rotation speed of 70r/min to obtain the organic acid activator.
Preparation example 4
The preparation example discloses a preparation method of an organic acid activator, which specifically comprises the following steps:
adding 3.86g of succinic acid, 3.41g of malic acid and 2.73g of sebacic acid into a stirrer, and stirring for 7min at the normal temperature and the rotation speed of 70r/min to obtain an organic acid activator; wherein the mass ratio of the succinic acid to the malic acid to the sebacic acid is 1.7:1.5: 1.2.
Preparation example 5
The preparation example discloses a preparation method of an organic acid activator, which specifically comprises the following steps:
adding 3.8g of succinic acid, 3.4g of malic acid and 2.8g of sebacic acid into a stirrer, and stirring for 7min at normal temperature and the rotation speed of 70r/min to obtain an organic acid activator; wherein the mass ratio of the succinic acid to the malic acid to the sebacic acid is 1.9:1.7: 1.4.
Preparation example 6
The preparation example discloses a preparation method of a surfactant, which specifically comprises the following steps:
adding 5g of triethanolamine and 5g of butyl acetate into a stirrer, and stirring for 5min at normal temperature and the rotation speed of 70r/min to obtain the surfactant.
Preparation example 7
The preparation example discloses a preparation method of a surfactant, which specifically comprises the following steps:
adding 5g of N-dodecyl alanine and 5g of EDTA disodium into a stirrer, and stirring for 5min at normal temperature and 70r/min to obtain the surfactant.
Preparation example 8
The preparation example discloses a preparation method of a surfactant, which specifically comprises the following steps:
adding 3g of butyl acetate, 4g of EDTA disodium and 3g of N-dodecyl alanine into a stirrer, and stirring for 7min at normal temperature and the rotating speed of 70r/min to obtain the surfactant.
Preparation example 9
The preparation example discloses a preparation method of a surfactant, which specifically comprises the following steps:
adding 4.69g of triethanolamine, 3.13g of butyl acetate and 2.18g of N-dodecyl alanine into a stirrer, and stirring for 7min at normal temperature and the rotating speed of 70r/min to obtain a surfactant; wherein the mass ratio of the triethanolamine to the butyl acetate is 1.5:1: 0.7.
Preparation example 10
The preparation example discloses a preparation method of a surfactant, which specifically comprises the following steps:
adding 4.15g of triethanolamine, 3.66g of butyl acetate and 2.19g of N-dodecyl alanine into a stirrer, and stirring for 7min at normal temperature and 70r/min to obtain a surfactant; wherein the mass ratio of the triethanolamine to the butyl acetate is 1.7:1.5: 0.9.
Preparation example 11
The preparation example discloses a preparation method of a film forming agent, which specifically comprises the following steps:
adding 5.88g of polyacrylamide, 2.94g of ethylene diamine tetramethylene sodium phosphate and 1.18g of polyethylene oxide into a stirrer, and stirring for 10min at normal temperature and at the rotating speed of 70r/min to obtain a film-forming agent; wherein the mass ratio of polyacrylamide to ethylene diamine tetramethylene sodium phosphate to polyethylene oxide is 1: 0.5: 0.2.
preparation example 12
The preparation example discloses a preparation method of a film forming agent, which specifically comprises the following steps:
adding 5.22g of polyacrylamide, 3.04g of ethylene diamine tetramethylene sodium phosphate and 1.74g of polyethylene oxide into a stirrer, and stirring for 10min at normal temperature and at the rotating speed of 70r/min to obtain a film-forming agent; wherein the mass ratio of polyacrylamide to ethylene diamine tetramethylene sodium phosphate to polyethylene oxide is 1.2: 0.7: 0.4.
preparation example 13
The preparation example discloses a preparation method of a film forming agent, which specifically comprises the following steps:
adding 5.5g of polyacrylamide, 3g of ethylene diamine tetramethylene sodium phosphate and 1.5g of polyethylene oxide into a stirrer, and stirring for 10min at normal temperature and at the rotating speed of 70r/min to obtain a film-forming agent; wherein the mass ratio of polyacrylamide to ethylene diamine tetramethylene sodium phosphate to polyethylene oxide is 1.1: 0.6: 0.3.
preparation example 14
The preparation example discloses a preparation method of a film forming agent, which specifically comprises the following steps:
adding 3g of polyacrylamide, 4g of ethylene diamine tetramethylene sodium phosphate and 3g of polyethylene oxide into a stirrer, and stirring for 10min at the normal temperature and the rotating speed of 70r/min to obtain a film-forming agent; wherein the mass ratio of polyacrylamide to ethylene diamine tetramethylene sodium phosphate to polyethylene oxide is 3: 4: 3.
preparation example 15
The difference between the present preparation example and preparation example 11 is that: the film forming agent is 10g of polyethylene glycol 600.
Examples
Examples 1 to 3
Embodiments 1 to 3 disclose a flux for wave soldering, the flux comprising the following raw materials by mass: 2-5% of an organic acid activator; 1.5 to 3.5 percent of surfactant; 0.5-1% of film-forming agent; 0.05 to 0.07 percent of corrosion inhibitor; the balance of carrier solvent.
The embodiment also discloses a manufacturing method of the soldering flux for wave soldering, which comprises the following steps:
step 1, mixing dipropylene glycol methyl ether, dipropylene glycol ethyl ether and butyl ether according to a mass ratio of 6: 3: 1, adding the mixture into a stirrer, stirring for 10min at the normal temperature and the rotating speed of 70r/min to obtain an alcohol ether solvent, heating the alcohol ether solvent to 60-70 ℃, and then mixing ethyl cellulose and the alcohol ether solvent according to the mass ratio of 1:6, stirring for 15min at the temperature of 60-70 ℃ and the rotating speed of 100r/min until the mixture is completely and uniformly dissolved to form a non-rosin carrier solvent;
step 2, adding a surfactant into a carrier solvent, stirring for 5min at the temperature of 60-70 ℃ and the rotating speed of 100r/min, adding a film forming agent and a corrosion inhibitor, and continuously stirring for 10min to obtain a mixed solution;
and 3, heating the mixed solution to the temperature of 100-145 ℃, adding an organic acid activator, and stirring for 5min under the condition that the rotating speed is 500r/min to obtain the wave soldering flux.
The raw materials and process parameters used in examples 1-3 are detailed in Table 1
TABLE 1
Example 4
The embodiment discloses a manufacturing method of a flux for wave soldering, which is different from the embodiment 1 in that: in the step 1, the addition amount of ethyl cellulose is 13.48g, the addition amount of dipropylene glycol methyl ether is 48.52g, the addition amount of dipropylene glycol ethyl ether is 24.26g, and the addition amount of butyl ether is 8.09 g; in the step 2, the addition amount of the surfactant is 2g, and the addition amount of the film forming agent is 0.6 g; in step 3, the amount of the organic acid activator added was 3 g.
Example 5
The embodiment discloses a manufacturing method of a soldering flux for wave soldering, which is different from the embodiment 1 in that: in the step 1, the addition amount of ethyl cellulose is 13.32g, the addition amount of dipropylene glycol methyl ether is 47.96g, the addition amount of dipropylene glycol ethyl ether is 23.98g, and the addition amount of butyl ether is 7.99 g; in the step 2, the addition amount of the surfactant is 2g, and the addition amount of the film forming agent is 0.7 g; in step 3, the amount of the organic acid activator added was 4 g.
Example 6
The embodiment discloses a manufacturing method of a soldering flux for wave soldering, which is different from the embodiment 1 in that: in the step 1, the addition amount of ethyl cellulose is 13.69g, the addition amount of dipropylene glycol methyl ether is 49.29g, the addition amount of dipropylene glycol ethyl ether is 24.65g, and the addition amount of butyl ether is 8.22 g; in step 2, 0.1g of hydroquinone antioxidant was also added.
Example 7
The embodiment discloses a manufacturing method of a flux for wave soldering, which is different from the embodiment 1 in that: in the step 1, the addition amount of ethyl cellulose is 13.66g, the addition amount of dipropylene glycol methyl ether is 49.19g, the addition amount of dipropylene glycol ethyl ether is 24.60g, and the addition amount of butyl ether is 8.20 g; in step 2, 0.3g of 2, 6-di-tert-butyl-p-cresol antioxidant was also added.
Example 8
The embodiment discloses a manufacturing method of a soldering flux for wave soldering, which is different from the embodiment 1 in that: in the step 1, the addition amount of ethyl cellulose is 13.68g, the addition amount of dipropylene glycol methyl ether is 49.24g, the addition amount of dipropylene glycol ethyl ether is 24.62g, and the addition amount of butyl ether is 8.21 g; in step 2, 0.1g of hydroquinone and 0.1g of catechol were also added.
Example 9
The manufacturing method of the soldering flux for wave soldering is different from the embodiment 1 in that: in step 3, the organic acid activator prepared in preparation example 4 is used as the organic acid activator.
Example 10
The manufacturing method of the soldering flux for wave soldering is different from the embodiment 1 in that: in step 3, the organic acid activator prepared in preparation example 5 is used as the organic acid activator.
Example 11
The manufacturing method of the soldering flux for wave soldering is different from the embodiment 1 in that: in step 2, the surfactant prepared in preparation example 9 was used as the surfactant.
Example 12
The manufacturing method of the soldering flux for wave soldering is different from the embodiment 1 in that: in step 2, the surfactant prepared in preparation example 10 is selected as the surfactant.
Example 13
The manufacturing method of the soldering flux for wave soldering is different from the embodiment 1 in that: in the step 1, the addition amount of ethyl cellulose is 13.29g, the addition amount of dipropylene glycol methyl ether is 47.86g, the addition amount of dipropylene glycol ethyl ether is 23.93g, and the addition amount of butyl ether is 7.97 g; in the step 2, the addition amount of the surfactant is 2g, the addition amount of the film forming agent is 0.7g, and 0.1g of hydroquinone and 0.1g of catechol are also added; in the step 3, the addition amount of the organic acid activator is 4 g; in the step 2, the surfactant prepared in the preparation example 10 is selected as the surfactant; the film-forming agent prepared in preparation example 13 is selected as the film-forming agent; in step 3, the organic acid activator prepared in preparation example 5 is used as the organic acid activator.
Comparative example
Comparative example 1
The manufacturing method of the soldering flux for wave soldering is different from the embodiment 1 in that: in the step 1, the addition amount of ethyl cellulose is 12.99g, the addition amount of dipropylene glycol methyl ether is 46.77g, the addition amount of dipropylene glycol ethyl ether is 23.39g, and the addition amount of butyl ether is 7.8 g; in the step 2, the addition amount of the surfactant is 1g, and the addition amount of the film forming agent is 1 g; in step 3, the amount of the organic acid activator added was 7 g.
Comparative example 2
The manufacturing method of the soldering flux for wave soldering is different from the embodiment 1 in that: in the step 1, the addition amount of ethyl cellulose is 13.35g, the addition amount of dipropylene glycol methyl ether is 48.06g, the addition amount of dipropylene glycol ethyl ether is 24.03g, and the addition amount of butyl ether is 8.01 g; in the step 2, the addition amount of the surfactant is 5g, and the addition amount of the film forming agent is 0.5 g; in step 3, the amount of the organic acid activator added was 1 g.
Comparative example 3
The manufacturing method of the soldering flux for wave soldering is different from the embodiment 1 in that: in the step 2, the film forming agent is added into the carrier solvent, stirred for 5min at the temperature of 60-70 ℃ and the rotating speed of 100r/min, then added with the surfactant and the corrosion inhibitor, and continuously stirred for 10min to obtain a mixed solution.
Comparative example 4
A manufacturing method of a soldering flux for wave soldering is different from that of embodiment 1 in that in step 1, 71.96g of isopropanol and 23.99g of butyl ether are mixed and added into a stirrer, and the mixture is stirred for 10min at the normal temperature and the rotating speed of 70r/min to obtain a common carrier solvent.
Comparative example 5
The manufacturing method of the soldering flux for wave soldering is different from the embodiment 1 in that: in the step 2, the film-forming agent prepared in preparation example 14 is selected as the film-forming agent.
Comparative example 6
The manufacturing method of the soldering flux for wave soldering is different from the embodiment 1 in that: in the step 2, the film-forming agent prepared in the preparation example 15 is selected as the film-forming agent.
Comparative example
Comparative example 1
A soldering flux for wave soldering is a commercial US MG CHEMICALS 837LFWS lead-free water-soluble soldering flux.
Comparative example 2
A flux for wave soldering selects a rosin flux sold in Shandong Beta chemical Co., Ltd No. 200.
Comparative example 3
A soldering flux for wave soldering selects a commercially available Evenst EV-901S liquid soldering flux.
Performance test
The fluxes prepared in examples 1 to 13, comparative examples 1 to 6 and comparative examples 1 to 3 were subjected to tests for testing the physical stability, spreading ratio, dryness, corrosion of copper mirror, corrosion of copper plate, insulation resistance after welding, oxidation resistance and the like under standard test conditions in accordance with the GB/T9491 standard:
the performance test standards are detailed in table 2.
TABLE 2
Specific test data of each performance test of examples 1 to 13, comparative examples 1 to 6 and comparative examples 1 to 3 are shown in tables 3 to 6.
TABLE 3
According to the performance detection data of the examples 1-3 and the comparative examples 1-3 in the table 3, the wave soldering flux prepared in the examples 1-3 has stable physical properties, smooth and mellow welding spots and good appearance; the splashing is small, and tin beads are not easy to generate; the expansion rate reaches the fluxing effect of the water-based soldering flux of the comparative example 1 and the rosin soldering flux of the comparative example 2; compared with the soldering flux of the comparative examples 1-3, the soldering flux prepared in the examples 1-3 has the advantages of good soldering effect, small corrosion residue, high insulation resistance after soldering, high reliability after soldering, good oxidation resistance, good performances in all aspects and wide application prospect.
TABLE 4
According to the performance test data of the examples 4 and 5 in the table 4, the component ratios among the organic acid activator, the surfactant and the film forming agent in the soldering flux are further defined in the examples 4 and 5 in the process of preparing the soldering flux, so that the soldering flux prepared in the examples 4 and 5 has better spreading rate and stability, the splashing condition is improved, and the oxidation resistance is more durable.
As can be seen from the performance testing data of examples 6-8 in Table 4, the addition of the antioxidant agent in examples 6-8 further improved the antioxidant performance of the fluxes prepared in examples 6-8 compared to the fluxes prepared in examples 1-3.
TABLE 5
According to the performance test data of the comparative examples 1 to 3 in the table 5, compared with the examples 1 to 3, in the process of preparing the soldering flux, the comparative examples 1 and 2 break through the component proportion range among the organic acid activator, the surfactant and the film forming agent and the unbalance of the combination proportion among the organic acid activator, the surfactant and the film forming agent in the examples 1 to 3, so that the performances of the soldering fluxes prepared in the comparative examples 1 and 2 are greatly influenced compared with the soldering fluxes prepared in the examples 1 to 3.
In the comparative example 1, the mass ratio of the organic acid activator to the surfactant to the film forming agent is 7:1:2, the content of the organic acid activator to the content of the film forming agent is too high, the content of the surfactant is too low, so that the corrosion of the soldering flux is too high, the residues after welding are too many and have very high corrosion, the insulation resistance of the welded surface is obviously reduced, the oxidation resistance is reduced, and the welded electronic element has larger potential safety hazards.
In the comparative example 2, the mass ratio of the organic acid activator to the surfactant to the film forming agent is 1:5:0.2, the content of the organic acid activator and the content of the film forming agent are too low, the content of the surfactant is too high, so that the stability of a soldering flux system is reduced, the soldering effect of the soldering flux is obviously reduced, the too low film forming agent is difficult to completely cover the surface of molten alloy liquid, and a welding spot is easy to oxidize and retract; the oxidation resistance and insulation of the soldered electronic component are reduced.
The film forming agent is added firstly and then the surfactant is added in the comparative example 3, the sequence of adding the surfactant firstly and then adding the film forming agent in the examples 1-3 is opposite, the film forming agent in the comparative example 3 cannot play a role in coating and blocking the organic acid activator, the organic acid activator and the surfactant are in contact reaction in advance, so that the activity of the organic acid activator is influenced, and the soldering assistant effect of the soldering flux is further influenced.
By comparing the performance test data of examples 1 to 3 and comparative examples 1 to 3, the inventors analyzed: according to the application, the organic acid activator, the surfactant and the film-forming agent are compounded according to a certain proportion and a certain adding sequence, and under the combined action of the three in a specific proportion, the good film-forming barrier property of the film-forming agent can fully wrap and block the organic acid activator, so that the direct contact between the organic acid activator and the metal surface is reduced at normal temperature, the corrosivity of the organic acid activator is reduced, and the activation stability of the organic acid activator is ensured; after the welding temperature is reached, the film forming agent shows activity, the wrapping and blocking effects on the organic acid disappear, the organic acid activator is in full contact with the surface of the metal to be welded under the assistance of the surfactant with stronger wetting capacity, the oxide layer on the surface of the metal to be welded is decomposed efficiently and quickly, and the strong fluxing property is shown; the film forming agent can form a complete protective film on the surface of the solder after welding to prevent the re-oxidation of the solder, so that the appearance of a welding spot is good, and the film forming agent can quickly solidify residues after high-temperature decomposition and prevent the continuous activation of an activating agent, thereby reducing the corrosivity of flux residues.
A soldering flux solution system formed by compounding the components in the soldering flux according to a specific ratio has better viscosity and expansibility, so that the splashing condition is good during wave soldering, and the formation of tin beads is reduced; the good viscosity and expansibility can not block a soldering flux spray head of wave soldering, and is beneficial to the expansion of solder, so that welding spots are smooth and mellow, the surface of the soldered board is clean and tidy, residues are less, and the subsequent long-term use of electronic and electric materials is not influenced.
The inventor finds that the surfactant, the film forming agent, the organic acid activator and the carrier solvent in the flux have good physical stability and excellent oxidation resistance under a proper combination ratio, and the stability and the oxidation resistance of the flux are greatly influenced after the content ratio of the components is changed; the components of the soldering flux cannot generate good synergistic effect, so that the soldering effect of the soldering flux is weakened, and the corrosion residue is increased.
In comparative example 4, the carrier solvent is a common solvent prepared by mixing isopropanol and butyl ether, and compared with the carrier solvent prepared by mixing dipropylene glycol methyl ether, dipropylene glycol ethyl ether and butyl ether according to the mass ratio of 6: 3: 1, mixing to obtain an alcohol ether solvent, and mixing ethyl cellulose and the alcohol ether solvent according to the mass ratio of 1:6 to obtain the carrier solvent, wherein the carrier solvent prepared by the method has better stability, promotes the full dissolution and blending of other components in the soldering flux, not only ensures that the soldering flux has good stability and oxidation resistance, but also promotes the spreading of solder and improves the soldering flux effect, and the carrier solvent is replaced by a common solvent in a comparative example 5, so that the stability and the oxidation resistance of the soldering flux prepared by the comparative example 5 are reduced.
The film forming agents prepared in preparation examples 14 and 15 are selected from comparative examples 5 and 6, the ratio of polyacrylamide, sodium ethylene diamine tetra-methylene phosphate and polyethylene oxide in the film forming agent prepared in preparation example 14 is beyond the range defined in examples 1-3, and the synergistic effect of polyacrylamide, sodium ethylene diamine tetra-methylene phosphate and polyethylene oxide is affected, so that the performance of the soldering flux prepared in comparative example 5 is reduced. In the preparation example 15, the polyethylene glycol 600 is selected as a film forming agent, the polyethylene glycol 600 cannot replace the film forming agent prepared in the application, and the coordination effect between the polyethylene glycol 600 and the organic acid active agent, the surfactant and the carrier solvent is greatly reduced, so that the performance of the soldering flux prepared in the comparative example 6 is reduced.
TABLE 6
According to the performance detection data of the examples 9 to 13 in the table 6, the organic acid activators prepared in the preparation examples 4 and 5 are adopted in the examples 9 and 10, the organic acid activators succinic acid, malic acid and sebacic acid in the preparation examples 4 and 5 are prepared by mixing (1.7-1.9) to (1.5-1.7) to (1.2-1.4) according to the mass ratio, the three acids are compounded according to a certain proportion range, the three acids can be well compatible, and have high reaction activity under the combined action, so that the soldering assistant effect of the soldering flux is further improved, and the soldering assistant effect of the soldering flux prepared in the examples 9 and 10 is improved compared with the soldering flux prepared in the examples 1 to 3.
The surfactants prepared in preparation examples 9 and 10 were used in examples 11 and 12, and the surfactants in preparation examples 9 and 10 were prepared from triethanolamine, butyl acetate and N-dodecylalanine in a mass ratio of (1.5-1.7) to (1-1.5): (0.7-0.9), reacting after mixing with an organic acid activator to generate a neutralization product, and rapidly decomposing the neutralization product at the welding temperature to regenerate organic acid and organic amine, so that the reactivity during organic acid welding is ensured, and the soldering assistant effect is promoted; after the welding is finished, the residual organic acid is neutralized by organic amine in the surfactant, so that the acidity of the residue is reduced, and the corrosion is reduced; the surfactant formed by mixing triethanolamine, butyl acetate and N-dodecylalanine in the preparation examples 9 and 10 has good compatibility with other components of the soldering flux, and has certain complexation, and the effect of a stabilizer can be achieved by matching with a film forming agent and a carrier solvent, so that the soldering flux prepared in the embodiments 11 and 12 has good soldering effect and structural stability.
In example 13, the organic acid activator obtained in preparation example 5, the surfactant obtained in preparation example 10, and the film-forming agent obtained in preparation example 13 were respectively selected and added with an antioxidant, so that the flux obtained in example 13 has an excellent flux effect, less corrosion residue, and excellent oxidation resistance and physical stability.
The above embodiments are preferred embodiments of the present application, and the protection scope of the present application is not limited by the above embodiments, so: equivalent changes in structure, shape and principle of the present application shall be covered by the protection scope of the present application.
Claims (8)
1. A flux for wave soldering, which is characterized in that: the material comprises the following raw materials in percentage by mass:
2-5% of an organic acid activator; 1.5 to 3.5 percent of surfactant; 0.5-1% of film-forming agent; 0.05 to 0.07 percent of corrosion inhibitor; the balance of carrier solvent;
wherein the organic acid activator is a mixture of two or more of succinic acid, adipic acid, malic acid and sebacic acid; the surfactant is a mixture of two or more of triethanolamine, butyl acetate, EDTA disodium and N-dodecyl alanine; the film forming agent is prepared from polyacrylamide, ethylene diamine tetramethylene sodium phosphate and polyethylene oxide according to the mass ratio of (1-1.2): (0.5-0.7): (0.2-0.4) mixing; the carrier solvent is prepared by mixing ethyl cellulose and an alcohol ether solvent according to the mass ratio of 1: 6.
2. The flux according to claim 1, wherein: the mass ratio of the organic acid activator to the surfactant to the film forming agent is (3-4): 2: (0.6-0.7).
3. The flux according to claim 1 or 2, wherein: the organic acid activator is prepared by mixing 1.7-1.9 mass percent of succinic acid, 1.5-1.7 mass percent of malic acid and 1.2-1.4 mass percent of sebacic acid.
4. The flux according to claim 1 or 2, wherein: the surfactant is prepared from triethanolamine, butyl acetate and N-dodecyl alanine according to the mass ratio of (1.5-1.7) to (1-1.5): (0.7-0.9) mixing.
5. The flux according to claim 1 or 2, wherein: the alcohol ether solvent is dipropylene glycol methyl ether, dipropylene glycol ethyl ether and butyl ether according to the mass ratio of 6: 3: 1, mixing to obtain the product.
6. The flux according to claim 1 or 2, wherein: the corrosion inhibitor is benzotriazole.
7. The flux according to claim 1 or 2, wherein: the material also comprises the following raw materials in percentage by mass: 0.1 to 0.3 percent of antioxidant, wherein the antioxidant is one or a mixture of 2, 6-di-tert-butyl-p-cresol, hydroquinone and catechol.
8. A method of making the flux for wave soldering according to any one of claims 1 to 7, wherein: the method comprises the following steps:
step 1, mixing ethyl cellulose and an alcohol ether solvent according to a mass ratio of 1:6, mixing, stirring at 60-70 ℃ until the mixture is completely and uniformly dissolved to form a non-rosin carrier solvent;
step 2, adding a surfactant into a carrier solvent, uniformly mixing, adding a film-forming agent and a corrosion inhibitor, and uniformly mixing to obtain a mixed solution;
and 3, heating the mixed solution to 100-145 ℃, adding an organic acid activator, and uniformly stirring to obtain the wave soldering flux.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116618778A (en) * | 2023-05-05 | 2023-08-22 | 广东剑鑫科技股份有限公司 | Welding process of efficient soldering flux |
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| CN116618778B (en) * | 2023-05-05 | 2023-12-05 | 广东剑鑫科技股份有限公司 | Welding process of efficient soldering flux |
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