CN115820140A - Wiping-free welding film and preparation method thereof - Google Patents
Wiping-free welding film and preparation method thereof Download PDFInfo
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- CN115820140A CN115820140A CN202211671696.1A CN202211671696A CN115820140A CN 115820140 A CN115820140 A CN 115820140A CN 202211671696 A CN202211671696 A CN 202211671696A CN 115820140 A CN115820140 A CN 115820140A
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Abstract
The invention relates to the technical field of welding films, and particularly discloses a wiping-free welding film, which comprises a welding flux layer, wherein adhesive film composite layers are arranged on two sides of the welding flux layer; the adhesive film composite layer comprises a base cloth layer, the modified impregnating compound is sprayed on the base cloth layer to form a space protective coating, and adhesive film modifiers are coated on two side surfaces of the space protective coating to form the adhesive film composite layer. The glue film composite layer is formed by matching a space protective coating and a glue film modifier together, and the modified impregnating compound in the space protective coating can be used as an intermediate bridge by optimizing the effect of taking modified bentonite as the space protective coating, so that on one hand, the temperature transmission is blocked, the high-temperature resistant effect of the product is improved, on the other hand, external molecules are prevented from entering a solder layer, the corrosion-resistant protection effect is improved, and the application efficiency of the glue film composite layer is enhanced.
Description
Technical Field
The invention relates to the technical field of welding films, in particular to a wiping-free welding film and a preparation method thereof.
Background
The film is a thin, soft, transparent sheet. Made of plastic, adhesive, rubber or other materials. The scientific interpretation of the film is: a 2-dimensional material formed by atomic, molecular or ionic deposition on a substrate surface. For example, optical films, composite films, superconducting films, polyester films, nylon films, plastic films, etc. The film is widely used in the industries of electronic and electric appliances, machinery, printing and the like. The welding film is used for wetting the surface of the welding position of the broken lead by the molten solder, and infiltrating into the butt joint of the broken ends of the lead to form a film layer with a smooth welding seam, so that the broken lead is connected, and the broken fine copper lead is effectively welded and repaired.
The welding film takes tin-lead solder with a melting point of 182-190 ℃ as a basic layer, is matched with the film layer for protection, can achieve a welding effect by melting and welding at the temperature of about 200 ℃, but the film layer has poor stain resistance and corrosion resistance, is easy to pollute and corrode, limits the protection efficiency of the basic layer, further influences the welding efficiency of the later solder, is difficult to coordinately improve the corrosion resistance and stain resistance of the film layer in the prior art, and reduces the use efficiency of products.
Disclosure of Invention
In view of the defects of the prior art, the present invention is directed to a wipe-free soldering film and a method for manufacturing the same, so as to solve the problems mentioned in the background art.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a wiping-free welding film, which comprises a welding flux layer, wherein glue film composite layers are arranged on two sides of the welding flux layer; the adhesive film composite layer comprises a base cloth layer, the modified impregnating compound is sprayed on the base cloth layer to form a space protective coating, and adhesive film modifying agents are coated on two side surfaces of the space protective coating to form the adhesive film composite layer;
wherein the adhesive film modifier comprises the following raw materials in parts by weight: 5-10 parts of wollastonite reconstituted nano silicon dioxide agent, 20-30 parts of ethanol solution, 3-5 parts of surface conditioning additive, 4-6 parts of epoxy resin and 4-7 parts of polyurethane adhesive;
the preparation method of the modified impregnating compound comprises the following steps:
s1: performing thermal dispersion improvement treatment on the bentonite for later use;
the specific improved treatment method comprises the following steps:
s11: performing heat treatment at 350-400 deg.C for 10-15min, and stopping heating at 45-55 deg.C at 2-5 deg.C/min;
s12: then sending the mixture into 5-7 times of hydrochloric acid solution with the mass fraction of 5% for uniform dispersion, and finally washing and drying;
s2: and (2) adding the bentonite of S1 into 20-30 parts of deionized water, then adding hydrochloric acid to adjust the pH value to 4.0, then adding 2-5 parts of sodium dodecyl sulfate, uniformly stirring, finally washing with water and drying to obtain the modified impregnating compound.
The inventor of the invention finds that the contact angle and the surface tension of the product are obviously poor under the conditions of acid and salt fog because the modified impregnating compound is not sprayed on the base cloth layer to form the interlayer protective coating, and meanwhile, the modified impregnating compound is replaced by bentonite and graphene, and an improved treatment method is not adopted in the preparation of the modified impregnating compound, so that the bentonite is directly operated by adopting the step S2, and the corrosion resistance and the stability of the product tend to be poor; therefore, the modified impregnating compound prepared by the method has the most remarkable improvement on the performance of the product.
Preferably, the solder layer is a tin-lead solder layer with the thickness of 0.2-0.4mm; the thickness of the modified film layer is 0.1-0.15mm.
Preferably, the preparation method of the adhesive film modifier comprises the following steps:
s101: adding 5-10 parts of polytetrafluoroethylene emulsion into 20-30 parts of ethanol, then adding 4-7 parts of rare earth composite nano silicon dioxide blending agent, and uniformly stirring for later use;
s102: adding wollastonite into the S01 product according to the weight ratio of 1:4, fully stirring, washing with water, and drying to obtain a wollastonite compound nano-silica agent;
s103: adding 5-10 parts of wollastonite reconstituted nano silicon dioxide agent into 20-30 parts of 25% ethanol solution by mass, then adding 3-5 parts of surface conditioning aid, 4-6 parts of epoxy resin and 4-7 parts of polyurethane adhesive, and continuously and fully stirring to obtain the adhesive film modifier.
Preferably, the mass fraction of the polytetrafluoroethylene emulsion is 10-20%.
Preferably, the stirring reaction temperature of S103 is 40-45 ℃, the stirring time is 55-65min, and the stirring speed is 550-600r/min.
Preferably, the rare earth composite nano silicon dioxide blending agent comprises the following raw materials in parts by weight:
5-10 parts of lanthanum chloride aqueous solution, 20-30 parts of deionized water, 1-5 parts of sodium alkyl sulfonate, 2-4 parts of chitosan and 6-10 parts of nano silicon dioxide.
The inventor of the invention finds that the rare earth composite nano-silica blending agent is directly replaced by nano-silica in the preparation of the wollastonite composite nano-silica blending agent, the lanthanum chloride aqueous solution, chitosan and sodium alkylsulfonate are not added in the preparation of the rare earth composite nano-silica blending agent, the corrosion resistance and the stain resistance of the product have a trend of becoming worse, only the wollastonite composite nano-silica blending agent prepared by the method has obvious performance effect, and the effect of the product is not obvious when the wollastonite composite nano-silica blending agent is replaced by other methods;
the inventor of the invention finds that in the preparation of the adhesive film modifier, the wollastonite raw material is replaced by graphene, the wollastonite is added, and simultaneously, bentonite accounting for 5 percent of the total amount of the wollastonite is added, so that the corrosion resistance of the product is obviously poor, the raw material selection in the preparation of the adhesive film modifier has specificity, the substitution and addition of other auxiliary raw materials have degradation tendency, and only the matching effect of the wollastonite and the nano-silica is most obvious;
according to the invention, the nano silicon dioxide and wollastonite replace traditional raw materials such as graphene and hydroxyapatite, and as the graphene sheet structure is adopted, the hydroxyapatite has a porous structure, so that the surface bearing area can be increased and the stain resistance effect can be enhanced, but the sheet structure is distributed, the contact area with an external acid-corrosion raw material is enhanced (the acid-corrosion substance of the hydroxyapatite Dan Yibei penetrates through the sheet structure), and the corrosion resistance effect is reduced on the contrary, so that the corrosion resistance and the stain resistance can be coordinately optimized;
preferably, the mass fraction of the lanthanum chloride aqueous solution is 10-15%.
Preferably, the preparation method of the surface conditioner comprises the following steps:
adding 2-5 parts of silane coupling agent KH560 into 5-10 parts of ethanol, adding 1-3 parts of ethyl silicate, 1-3 parts of triethylene glycol dimethacrylate and 2-6 parts of castor oil, and fully stirring to obtain the surface conditioning aid.
The inventor of the invention also finds that the silane coupling agent KH560 is not added in the preparation of the surface conditioning aid, the change trend of the stain resistance and the corrosion resistance of water, a membrane contact angle and surface tension is the largest, the silane coupling agent KH560 plays a leading role in the surface conditioning aid, and the addition of the ethyl silicate and the triethylene glycol dimethacrylate can coordinate with the silane coupling agent KH560 to jointly enhance the stain resistance and the corrosion resistance of the product; in addition, the cellulose acetate is additionally added, although the stain resistance can be improved under the conventional conditions, under the acid and salt fog conditions, the stain resistance of the product is more obviously deteriorated, and the stain resistance and corrosion resistance of the product cannot be coordinately improved, so that the preparation of the surface conditioning aid only adopts the raw material proportioning performance of the surface conditioning aid provided by the invention with the best effect, and adopts other raw materials to match, and the corrosion resistance and stain resistance of the product are difficult to coordinately improved.
The invention also provides a preparation method of the wiping-free welding film, which comprises the following steps:
the method comprises the following steps: spraying the modified impregnating compound on a base cloth layer to form a space protective coating, coating adhesive film modifying agents on two side surfaces of the space protective coating to form an adhesive film modified layer, and drying for 1-2 hours at the pressure of 5-10MPa and the temperature of 35-40 ℃ to obtain an adhesive film composite layer;
step two: and finally coating adhesive film composite layers on two sides of the tin-lead solder layer to form the wiping-free welding film.
Preferably, the thickness of the interlayer protective coating is 0.1-0.3mm, and the thickness of the adhesive film modification layer is 0.3-0.6mm.
Compared with the prior art, the invention has the following beneficial effects:
1. the glue film composite layer is formed by matching a space protective coating and a glue film modifier together, the modified impregnating compound in the space protective coating adopts bentonite for heat treatment firstly, and then is cooled at constant temperature, so that the lamellar structure of the glue film composite layer is expanded, the lamellar spacing is improved, and then the modified impregnating compound is dispersed and activated in hydrochloric acid solution and sodium dodecyl sulfate, so that the dispersity and the activity of the bentonite are improved, the modified bentonite is optimized to be used as the space protective coating to be used as an intermediate bridge, on one hand, the temperature transmission is blocked, the high temperature resistance effect of a product is improved, on the other hand, external molecules are blocked from entering a solder layer, the corrosion resistance protection effect is improved, and the application efficiency of the glue film composite layer is enhanced;
2. the adhesive film modifier adopts wollastonite to compound nano-silica agent, ethanol solution, surface conditioning aid and other raw materials, and forms an adhesive film modified layer through adhesive coating, the wollastonite has a needle-shaped structure, on one hand, the adhesive film modifier plays a role in reinforcing, meanwhile, the nano-silica has a spherical structure with a high specific surface area, the wollastonite can be borne in the nano-silica structure and arranged in a needle shape, stains are difficult to stay on the surface of a product, meanwhile, the nano-silica is cooperated with the wollastonite, the surface of the product can be reinforced and filled, the surface compactness is enhanced, and the product corrosion resistance efficiency is improved;
the nano-silica is subjected to raw material optimization modification in the rare earth composite nano-silica blending agent, and the interface of the nano-silica is enhanced through the matching of sodium alkylsulfonate, chitosan and lanthanum chloride aqueous solution, so that the synergistic effect of wollastonite in compounding the nano-silica is optimized and improved, the corrosion resistance and stain resistance effects of the product are improved, and the dual-functionalization effect of the product is enhanced;
3. the surface conditioning agent adopts a silane coupling agent, modifies the interface of raw materials of the product, optimizes wollastonite to re-condition the nano-silica agent by the synergistic effect of the ethyl silicate, the triethylene glycol dimethacrylate and the castor oil, reduces the low surface energy of the wollastonite, ensures that stains are difficult to attach, further enhances the stain resistance effect of the product, and simultaneously re-conditions the nano-silica agent by the optimized wollastonite to coordinate and enhance the effect.
4. In the bentonite thermal dispersion improvement treatment, firstly, the sheet layer is expanded through thermal treatment at 350-400 ℃, then, the temperature is reduced to 45-55 ℃ at the speed of 2-5 ℃/min, and the bentonite receives a mild thermal cooling effect by adopting constant speed cooling, so that the expanded sheet layer bentonite is not easy to shrink, the space between protective sheets is maximized, the bentonite is uniformly dispersed by hydrochloric acid solution at 45-55 ℃, the activity degree and the dispersibility are optimized in the optimal space between protective sheets, and finally, the aqueous solution of hydrochloric acid and sodium dodecyl sulfate is further modified and optimized, and the application effect of the modified impregnating compound can be obviously enhanced.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
In the wiping-free soldering film of the embodiment, the soldering film includes a solder layer, and adhesive film composite layers are disposed on two sides of the solder layer; the adhesive film composite layer comprises a base cloth layer, the modified impregnating compound is sprayed on the base cloth layer to form a space protective coating, and adhesive film modifiers are coated on two side surfaces of the space protective coating to form the adhesive film composite layer;
wherein the adhesive film modifier comprises the following raw materials in parts by weight: 5-10 parts of wollastonite reconstituted nano silicon dioxide agent, 20-30 parts of ethanol solution, 3-5 parts of surface conditioning additive, 4-6 parts of epoxy resin and 4-7 parts of polyurethane adhesive;
the preparation method of the modified impregnating compound comprises the following steps:
s1: performing thermal dispersion improvement treatment on the bentonite for later use;
the specific improved treatment method comprises the following steps:
s11: performing heat treatment at 350-400 deg.C for 10-15min, and stopping heating at 45-55 deg.C at 2-5 deg.C/min;
s12: then sending the mixture into 5-7 times of hydrochloric acid solution with the mass fraction of 5% for uniform dispersion, and finally washing and drying;
s2: and (2) adding the bentonite of S1 into 20-30 parts of deionized water, then adding hydrochloric acid to adjust the pH value to 4.0, then adding 2-5 parts of sodium dodecyl sulfate, uniformly stirring, finally washing with water and drying to obtain the modified impregnating compound.
The solder layer of the embodiment is a tin-lead solder layer, and the thickness is 0.2-0.4mm; the thickness of the modified film layer is 0.1-0.15mm.
The preparation method of the adhesive film modifier comprises the following steps:
s101: adding 5-10 parts of polytetrafluoroethylene emulsion into 20-30 parts of ethanol, then adding 4-7 parts of rare earth composite nano silicon dioxide blending agent, and uniformly stirring for later use;
s102: adding wollastonite into the S101 product according to the weight ratio of 1:4, fully stirring, washing with water, and drying to obtain a wollastonite compound nano silicon dioxide agent;
s103: adding 5-10 parts of wollastonite reconstituted nano silicon dioxide agent into 20-30 parts of 25% ethanol solution by mass, then adding 3-5 parts of surface conditioning aid, 4-6 parts of epoxy resin and 4-7 parts of polyurethane adhesive, and continuously and fully stirring to obtain the adhesive film modifier.
The mass fraction of the polytetrafluoroethylene emulsion in this example is 10-20%.
In the embodiment, the stirring reaction temperature of S103 is 40-45 ℃, the stirring time is 55-65min, and the stirring speed is 550-600r/min.
The rare earth composite nano silicon dioxide blending agent comprises the following raw materials in parts by weight:
5-10 parts of lanthanum chloride aqueous solution, 20-30 parts of deionized water, 1-5 parts of sodium alkyl sulfonate, 2-4 parts of chitosan and 6-10 parts of nano silicon dioxide.
The mass fraction of the lanthanum chloride aqueous solution in the embodiment is 10-15%.
The preparation method of the surface conditioner of the embodiment comprises the following steps:
adding 2-5 parts of silane coupling agent KH560 into 5-10 parts of ethanol, adding 1-3 parts of ethyl silicate, 1-3 parts of triethylene glycol dimethacrylate and 2-6 parts of castor oil, and fully stirring to obtain the surface conditioning aid.
The method for preparing a wipe-free soldering film of the embodiment comprises the following steps:
the method comprises the following steps: spraying a modified impregnating compound on a base cloth layer to form a space protective coating, coating adhesive film modifying agents on two side surfaces of the space protective coating to form an adhesive film modified layer, and drying for 1-2 hours at the pressure of 5-10MPa and the temperature of 35-40 ℃ to obtain an adhesive film composite layer;
step two: and finally coating adhesive film composite layers on two sides of the tin-lead solder layer to form the wiping-free welding film.
The thickness of the inter-layer protective coating in this embodiment is 0.1-0.3mm, and the thickness of the adhesive film modified layer is 0.3-0.6mm.
Example 1.
In the wiping-free soldering film of the embodiment, the soldering film includes a solder layer, and adhesive film composite layers are disposed on two sides of the solder layer; the adhesive film composite layer comprises a base cloth layer, the modified impregnating compound is sprayed on the base cloth layer to form a space protective coating, and adhesive film modifiers are coated on two side surfaces of the space protective coating to form the adhesive film composite layer;
wherein the adhesive film modifier comprises the following raw materials in parts by weight: 5-10 parts of wollastonite reconstituted nano silicon dioxide agent, 20-30 parts of ethanol solution, 3-5 parts of surface conditioning additive, 4-6 parts of epoxy resin and 4-7 parts of polyurethane adhesive;
the preparation method of the modified impregnating compound comprises the following steps:
s1: performing thermal dispersion improvement treatment on the bentonite for later use;
the specific improved treatment method comprises the following steps:
s11: performing heat treatment at 350 deg.C for 10min, and stopping at 45 deg.C at 2 deg.C/min;
s12: then sending the mixture into 5 times of hydrochloric acid solution with the mass fraction of 5% for uniform dispersion, and finally washing and drying;
s2: and (2) adding the bentonite of the S1 into 20 parts of deionized water, then adding hydrochloric acid to adjust the pH value to 4.0, then adding 2 parts of sodium dodecyl sulfate, uniformly stirring, finally washing and drying to obtain the modified impregnating compound.
The solder layer of the embodiment is a tin-lead solder layer, and the thickness is 0.2mm; the thickness of the modified film layer is 0.1mm.
The preparation method of the adhesive film modifier comprises the following steps:
s101: adding 5 parts of polytetrafluoroethylene emulsion into 20 parts of ethanol, then adding 4 parts of rare earth composite nano silicon dioxide blending agent, and uniformly stirring for later use;
s102: adding wollastonite into the S101 product according to the weight ratio of 1:4, fully stirring, washing with water, and drying to obtain a wollastonite compound nano silicon dioxide agent;
s103: adding 5-10 parts of wollastonite reconstituted nano-silica agent into 20 parts of 25% ethanol solution by mass, then adding 3 parts of surface conditioning aid, 4 parts of epoxy resin and 4 parts of polyurethane adhesive, and continuously and fully stirring to obtain the adhesive film modifier.
The polytetrafluoroethylene emulsion of this example was 10% by mass.
In the present example, the stirring reaction temperature of S103 is 40 ℃, the stirring time is 55min, and the stirring rotation speed is 550r/min.
The rare earth composite nano silicon dioxide blending agent comprises the following raw materials in parts by weight:
5 parts of lanthanum chloride aqueous solution, 20 parts of deionized water, 1 part of sodium alkyl sulfonate, 2 parts of chitosan and 6 parts of nano silicon dioxide.
The lanthanum chloride aqueous solution of this example was 10% by mass.
The preparation method of the surface conditioner in this embodiment is as follows:
adding 2 parts of silane coupling agent KH560 into 5 parts of ethanol, adding 1 part of ethyl silicate, 1 part of triethylene glycol dimethacrylate and 2 parts of castor oil, and fully stirring to obtain the surface conditioning aid.
The method for preparing a wipe-free soldering film of the embodiment comprises the following steps:
the method comprises the following steps: spraying a modified impregnating compound on a base fabric layer to form a space protective coating, coating adhesive film modifying agents on two side surfaces of the space protective coating to form an adhesive film modified layer, and drying for 1h at the pressure of 5MPa and the temperature of 35 ℃ to obtain an adhesive film composite layer;
step two: finally, coating adhesive film composite layers on two sides of the tin-lead solder layer to form the wiping-free welding film.
The thickness of the inter-layer protective coating in this example is 0.1mm, and the thickness of the adhesive film modified layer is 0.3mm.
Example 2.
In the wiping-free soldering film of the present embodiment, the soldering film includes a solder layer, and adhesive film composite layers are disposed on two sides of the solder layer; the adhesive film composite layer comprises a base cloth layer, the modified impregnating compound is sprayed on the base cloth layer to form a space protective coating, and adhesive film modifiers are coated on two side surfaces of the space protective coating to form the adhesive film composite layer;
wherein the adhesive film modifier comprises the following raw materials in parts by weight: 10 parts of wollastonite re-regulating nano silicon dioxide agent, 30 parts of ethanol solution, 5 parts of surface regulating agent, 6 parts of epoxy resin and 7 parts of polyurethane adhesive;
the preparation method of the modified impregnating compound comprises the following steps:
s1: performing thermal dispersion improvement treatment on the bentonite for later use;
the specific improved treatment method comprises the following steps:
s11: performing heat treatment at 400 deg.C for 15min, and stopping at 55 deg.C at a speed of 5 deg.C/min;
s12: then sending the mixture into 7 times of hydrochloric acid solution with the mass fraction of 5% for uniform dispersion, and finally washing and drying;
s2: and (2) adding the bentonite of S1 into 30 parts of deionized water, then adding hydrochloric acid to adjust the pH value to 4.0, then adding 5 parts of sodium dodecyl sulfate, uniformly stirring, finally washing and drying to obtain the modified impregnating compound.
The solder layer of the embodiment is a tin-lead solder layer, and the thickness is 0.4mm; the thickness of the modified film layer is 0.15mm.
The preparation method of the adhesive film modifier comprises the following steps:
s101: adding 10 parts of polytetrafluoroethylene emulsion into 30 parts of ethanol, then adding 7 parts of rare earth composite nano silicon dioxide blending agent, and uniformly stirring for later use;
s102: adding wollastonite into the S101 product according to the weight ratio of 1:4, fully stirring, washing with water, and drying to obtain a wollastonite compound nano silicon dioxide agent;
s103: adding 10 parts of wollastonite compound nano silicon dioxide agent into 30 parts of 25% ethanol solution by mass, then adding 5 parts of surface conditioning aid, 6 parts of epoxy resin and 7 parts of polyurethane adhesive, and continuously and fully stirring to obtain the adhesive film modifier.
The polytetrafluoroethylene emulsion of this example was 20% by mass.
In the present embodiment, the stirring reaction temperature of S103 is 45 ℃, the stirring time is 65min, and the stirring speed is 600r/min.
The rare earth composite nano silicon dioxide blending agent comprises the following raw materials in parts by weight:
10 parts of lanthanum chloride aqueous solution, 30 parts of deionized water, 5 parts of sodium alkylsulfonate, 4 parts of chitosan and 10 parts of nano silicon dioxide.
The mass fraction of the lanthanum chloride aqueous solution in this example was 10 to 15%.
The preparation method of the surface conditioner in this embodiment is as follows:
adding 5 parts of silane coupling agent KH560 into 10 parts of ethanol, adding 3 parts of ethyl silicate, 3 parts of triethylene glycol dimethacrylate and 6 parts of castor oil, and fully stirring to obtain the surface conditioning aid.
The preparation method of the wipe-free soldering film of the embodiment comprises the following steps:
the method comprises the following steps: spraying the modified impregnating compound on a base cloth layer to form a space protective coating, coating adhesive film modifying agents on two side surfaces of the space protective coating to form an adhesive film modified layer, and drying for 2 hours at the pressure of 10MPa and the temperature of 40 ℃ to obtain an adhesive film composite layer;
step two: and finally coating adhesive film composite layers on two sides of the tin-lead solder layer to form the wiping-free welding film.
The thickness of the inter-layer protective coating in this example is 0.3mm, and the thickness of the adhesive film modified layer is 0.6mm.
Example 3.
In the wiping-free soldering film of the embodiment, the soldering film includes a solder layer, and adhesive film composite layers are disposed on two sides of the solder layer; the adhesive film composite layer comprises a base cloth layer, the modified impregnating compound is sprayed on the base cloth layer to form a space protective coating, and adhesive film modifiers are coated on two side surfaces of the space protective coating to form the adhesive film composite layer;
wherein the adhesive film modifier comprises the following raw materials in parts by weight: 7.5 parts of wollastonite reconstituted nano silicon dioxide agent, 25 parts of ethanol solution, 4 parts of surface conditioning additive, 5 parts of epoxy resin and 5.5 parts of polyurethane adhesive;
the preparation method of the modified impregnating compound comprises the following steps:
s1: performing thermal dispersion improvement treatment on the bentonite for later use;
the specific improved treatment method comprises the following steps:
s11: carrying out heat treatment at 375 deg.C for 12.5min, and stopping heating at 50 deg.C at 3.5 deg.C/min;
s12: then sending the mixture into 6 times of hydrochloric acid solution with the mass fraction of 5% for uniform dispersion, and finally washing and drying;
s2: and (2) adding the bentonite of the S1 into 25 parts of deionized water, then adding hydrochloric acid to adjust the pH value to 4.0, then adding 3.5 parts of sodium dodecyl sulfate, uniformly stirring, finally washing with water, and drying to obtain the modified impregnating compound.
The solder layer of the embodiment is a tin-lead solder layer with the thickness of 0.3mm; the thickness of the modified film layer is 0.12mm.
The preparation method of the adhesive film modifier comprises the following steps:
s101: adding 7.5 parts of polytetrafluoroethylene emulsion into 25 parts of ethanol, then adding 5.5 parts of rare earth composite nano silicon dioxide blending agent, and uniformly stirring for later use;
s102: adding wollastonite into the S101 product according to the weight ratio of 1:4, fully stirring, washing with water, and drying to obtain a wollastonite compound nano silicon dioxide agent;
s103: adding 7.5 parts of wollastonite reconstituted nano-silica agent into 25 parts of 25 mass percent ethanol solution, then adding 4 parts of surface conditioning aid, 5 parts of epoxy resin and 5.5 parts of polyurethane adhesive, and continuously and fully stirring to obtain the adhesive film modifier.
The polytetrafluoroethylene emulsion of this example was 15% by mass.
In this example, the stirring reaction temperature of S103 was 42.5 deg.C, the stirring time was 60min, and the stirring speed was 570r/min.
The rare earth composite nano silicon dioxide blending agent comprises the following raw materials in parts by weight:
7.5 parts of lanthanum chloride aqueous solution, 25 parts of deionized water, 3 parts of sodium alkyl sulfonate, 3 parts of chitosan and 8 parts of nano silicon dioxide.
The lanthanum chloride aqueous solution of this example had a mass fraction of 12.5%.
The preparation method of the surface conditioner in this embodiment is as follows:
adding 3.5 parts of silane coupling agent KH560 into 7.5 parts of ethanol, adding 2 parts of ethyl silicate, 2 parts of triethylene glycol dimethacrylate and 4 parts of castor oil, and fully stirring to obtain the surface conditioning aid.
The method for preparing a wipe-free soldering film of the embodiment comprises the following steps:
the method comprises the following steps: spraying a modified impregnating compound on a base cloth layer to form a space protective coating, coating adhesive film modifiers on two side faces of the space protective coating to form an adhesive film modified layer, and drying at the pressure of 7.5MPa and the temperature of 37.5 ℃ for 1.5 hours to obtain an adhesive film composite layer;
step two: and finally coating adhesive film composite layers on two sides of the tin-lead solder layer to form the wiping-free welding film.
The thickness of the inter-layer protective coating in this example is 0.2mm, and the thickness of the adhesive film modified layer is 0.45mm.
Comparative example 1.
The difference from the example 3 is that the modified impregnating compound is not sprayed on the base fabric layer to form the interlayer protective coating.
Comparative example 2.
The difference from example 3 is that bentonite is used instead of the modified sizing agent.
Comparative example 3.
The difference from the example 3 is that the bentonite in the modified impregnating compound is replaced by graphene.
Comparative example 4.
Different from the example 3, the modified impregnating compound was prepared without using an improved treatment method, and the bentonite was directly subjected to the step S2.
Comparative example 5.
Different from the embodiment 3, in the preparation of the adhesive film modifier, the wollastonite raw material is replaced by graphene.
Comparative example 6.
The difference from the example 3 is that bentonite accounting for 5 percent of the total amount of the wollastonite is added at the same time of adding the wollastonite in the preparation of the adhesive film modifier.
Comparative example 7.
Different from the embodiment 3, the rare earth composite nano silicon dioxide blending agent in the preparation of the wollastonite compound nano silicon dioxide agent is directly replaced by nano silicon dioxide.
Comparative example 8.
Different from the embodiment 3, the preparation of the rare earth composite nano silicon dioxide blending agent does not add lanthanum chloride aqueous solution and chitosan.
Comparative example 9.
Different from the example 3, the preparation of the rare earth composite nano silicon dioxide blending agent does not add sodium alkyl sulfonate.
Comparative example 10.
Different from the embodiment 3, the tetrafluoroethylene emulsion is not added in the preparation of the wollastonite compound nano silicon dioxide agent.
Comparative example 11.
Different from the example 3, no surface conditioning agent is added in the preparation of the adhesive film modifier.
The products of examples 1-3 and comparative examples 1-11 were placed in a salt spray of 6% and 3% acid for 24h under conventional conditions, and the results of the property measurements were as follows
From examples 1 to 3 and comparative examples 1 to 11,
the product of embodiment 3 of the invention has excellent water and film contact angles and surface tension, the product has excellent stain resistance, the surface tension of the product is effectively reduced, stains are not easy to adhere, and meanwhile, the product still has excellent stain resistance and strong corrosion resistance stability under the corrosion conditions of acid and salt mist;
it is seen from comparative examples 1-4 and example 3 that the modified impregnating compound is not sprayed on the base cloth layer to form the interlayer protective coating, the contact angle and the surface tension of the product are obviously reduced under the conditions of acid and salt fog, meanwhile, the modified impregnating compound is replaced by bentonite and graphene, and an improved treatment method is not adopted in the preparation of the modified impregnating compound, the bentonite is directly operated by the step S2, and the corrosion resistance and the stability of the product tend to be reduced; therefore, the modified impregnating compound prepared by the method has the most obvious improvement on the performance of the product;
from comparative examples 5-6, it is seen that, in the preparation of the adhesive film modifier, the wollastonite raw material is replaced by graphene, and the wollastonite is added, and simultaneously, bentonite accounting for 5% of the total amount of the wollastonite is added, so that the corrosion resistance of the product is remarkably poor, the raw material selection in the preparation of the adhesive film modifier has specificity, the substitution and addition of other raw materials are poor, and only the collocation effect of the wollastonite and the nano-silica is most remarkable;
from comparative examples 7-10, it is seen that the rare earth composite nano-silica blending agent in the preparation of wollastonite reconstituted nano-silica agent is directly replaced by nano-silica, and lanthanum chloride aqueous solution, chitosan and sodium alkylsulfonate are not added in the preparation of the rare earth composite nano-silica blending agent, so that the corrosion resistance and stain resistance of the product tend to be poor, only the wollastonite reconstituted nano-silica agent prepared by the method of the present invention has significant performance effect, and the other methods are not used for replacing the wollastonite reconstituted nano-silica agent as the effect of the present invention is significant;
it is seen from comparative examples 1, 5 and 11 and example 3 that the surface conditioner is not added in the preparation of the adhesive film modifier, the corrosion resistance stability of the product is remarkably deteriorated, the conditions of acid and salt fog are poor, the contact angle and the surface tension both have a tendency of remarkably deteriorated, and the surface conditioner has a remarkable improvement effect on the pollution resistance and corrosion resistance stability of the product;
based on the tests, the invention finds that the surface conditioning agent has a larger influence tendency on the performance of the product, and based on the influence tendency, the invention further explores the product.
The preparation method of the surface conditioning aid comprises the following steps:
adding 3.5 parts of silane coupling agent KH560 into 7.5 parts of ethanol, adding 2 parts of ethyl silicate, 2 parts of triethylene glycol dimethacrylate and 4 parts of castor oil, and fully stirring to obtain the surface conditioning aid.
Experimental example 1.
The surface conditioner was prepared without adding the silane coupling agent KH560, as in example 3.
Experimental example 2.
The surface conditioner was prepared as in example 3 except that no ethyl silicate was added.
Experimental example 3.
The surface conditioner was prepared as in example 3 except that triethylene glycol dimethacrylate was not added.
Experimental example 4.
As in example 3, except that cellulose acetate was also added to the surface conditioner preparation.
As can be seen from the experimental examples 1-3, the silane coupling agent KH560 is not added in the preparation of the surface conditioning aid, the change trend of the stain resistance and the corrosion resistance of water, a membrane contact angle and surface tension is the largest, the silane coupling agent KH560 plays a leading role in the surface conditioning aid, and the addition of the ethyl silicate and the triethylene glycol dimethacrylate can coordinate with the silane coupling agent KH560 to jointly enhance the stain resistance and the corrosion resistance of the product;
as can be seen from the experimental example 4, in addition, the cellulose acetate is additionally added, although the stain resistance can be improved under the conventional conditions, under the acid and salt fog conditions, the stain resistance of the product is more obviously deteriorated, and the stain resistance and corrosion resistance of the product cannot be coordinately improved, so that the surface conditioning agent has the best effect only by adopting the raw material proportioning performance of the surface conditioning agent, and the corrosion resistance and stain resistance of the product are difficult to coordinately improved by adopting the matching of other raw materials.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present specification describes embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and it is to be understood that all embodiments may be combined as appropriate by one of ordinary skill in the art to form other embodiments as will be apparent to those of skill in the art from the description herein.
Claims (10)
1. A wiping-free welding film is characterized by comprising a welding flux layer, wherein glue film composite layers are arranged on two sides of the welding flux layer; the adhesive film composite layer comprises a base cloth layer, the modified impregnating compound is sprayed on the base cloth layer to form a space protective coating, and adhesive film modifying agents are coated on two side surfaces of the space protective coating to form the adhesive film composite layer;
wherein the adhesive film modifier comprises the following raw materials in parts by weight: 5-10 parts of wollastonite readjusting nano silicon dioxide agent, 20-30 parts of ethanol solution, 3-5 parts of surface conditioning aid, 4-6 parts of epoxy resin and 4-7 parts of polyurethane adhesive;
the preparation method of the modified impregnating compound comprises the following steps:
s1: performing thermal dispersion improvement treatment on the bentonite for later use;
s2: and (2) adding the bentonite of S1 into 20-30 parts of deionized water, then adding hydrochloric acid to adjust the pH value to 4.0, then adding 2-5 parts of sodium dodecyl sulfate, uniformly stirring, finally washing with water and drying to obtain the modified impregnating compound.
2. The wipe-free solder film according to claim 1, wherein the solder layer is a tin-lead solder layer having a thickness of 0.2 to 0.4mm; the thickness of the modified film layer is 0.1-0.15mm.
3. The wiping-free welding film as claimed in claim 1, wherein the adhesive film modifier is prepared by the following steps:
s101: adding 5-10 parts of lanthanum chloride aqueous solution into 20-30 parts of deionized water, then adding 1-5 parts of sodium alkylsulfonate and 2-4 parts of chitosan, uniformly stirring, finally adding 6-10 parts of nano silicon dioxide, and continuously and fully mixing to obtain a rare earth composite nano silicon dioxide blending agent;
s102: adding 5-10 parts of polytetrafluoroethylene emulsion into 20-30 parts of ethanol, then adding 4-7 parts of rare earth composite nano silicon dioxide blending agent, and uniformly stirring for later use;
s103: adding wollastonite into the S02 product according to the weight ratio of 1:4, fully stirring, washing with water, and drying to obtain a wollastonite reconditioned nano-silica agent;
s104: adding 5-10 parts of wollastonite reconstituted nano silicon dioxide agent into 20-30 parts of 25% ethanol solution by mass, then adding 3-5 parts of surface conditioning aid, 4-6 parts of epoxy resin and 4-7 parts of polyurethane adhesive, and continuously and fully stirring to obtain the adhesive film modifier.
4. The wiping-free soldering film as claimed in claim 3, wherein the polytetrafluoroethylene emulsion is present in an amount of 10 to 20% by mass.
5. The wiping-free solder film as claimed in claim 3, wherein the temperature of the stirring reaction of S104 is 40-45 ℃, the stirring time is 55-65min, and the stirring rotation speed is 550-600r/min.
6. The wiping-free soldering film as claimed in claim 3, wherein the aqueous solution of lanthanum chloride is present in an amount of 10 to 15% by mass.
7. The wipe-free soldering film according to claim 3, wherein the surface conditioner is prepared by:
adding 2-5 parts of silane coupling agent KH560 into 5-10 parts of ethanol, adding 1-3 parts of ethyl silicate, 1-3 parts of triethylene glycol dimethacrylate and 2-6 parts of castor oil, and fully stirring to obtain the surface conditioning aid.
8. The wipe-free soldering film according to claim 1, wherein the bentonite thermal dispersion improving treatment method comprises:
s11: performing heat treatment at 350-400 deg.C for 10-15min, and stopping heating at 45-55 deg.C at 2-5 deg.C/min;
s12: and then sending the mixture into 5-7 times of hydrochloric acid solution with the mass fraction of 5% to be uniformly dispersed, and finally washing and drying the mixture.
9. A method for preparing a wipe-free solder film according to any of claims 1 to 8, comprising the steps of:
the method comprises the following steps: spraying a modified impregnating compound on a base cloth layer to form a space protective coating, coating adhesive film modifying agents on two side surfaces of the space protective coating to form an adhesive film modified layer, and drying for 1-2 hours at the pressure of 5-10MPa and the temperature of 35-40 ℃ to obtain an adhesive film composite layer;
step two: finally, coating adhesive film composite layers on two sides of the tin-lead solder layer to form the wiping-free welding film.
10. The method for preparing a wipe-free soldering film according to claim 9, wherein the thickness of the interlayer protecting layer is 0.1-0.3mm, and the thickness of the adhesive film modifying layer is 0.3-0.6mm.
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