CN109971324B - High-temperature-resistant hole sealing agent and hole sealing method - Google Patents

High-temperature-resistant hole sealing agent and hole sealing method Download PDF

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CN109971324B
CN109971324B CN201910209062.6A CN201910209062A CN109971324B CN 109971324 B CN109971324 B CN 109971324B CN 201910209062 A CN201910209062 A CN 201910209062A CN 109971324 B CN109971324 B CN 109971324B
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CN109971324A (en
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唐鹏
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Huizhou Recepho Science & Technology Co ltd
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Abstract

A high-temperature resistant hole sealing agent does not contain any heavy metal such as chromic acid, cobaltic acid and the like, so that the problem that a flexible circuit board is poor in contact resistance and weldability caused by using chromic acid and cobaltic acid in the past is solved, wherein under the condition that the joint pressure is not less than 10g/m square meter, the change of the contact resistance before and after treatment of the high-temperature resistant hole sealing agent is not more than 5 percent (less than 0.05m omega), and the high-frequency performance is as follows: the standing-wave ratio is less than or equal to 1.03, the attenuation is less than or equal to 0.08db, and the separation force is reduced by more than 35% before and after treatment; in addition, the flexible printed circuit board can resist the high temperature of 280 ℃, can be continuously supplemented for use, is harmless to the environment and human bodies, can be degraded automatically, can greatly improve the salt spray resistance and the high temperature resistance of the gold-plated flexible printed circuit board, and particularly can improve the acid sweat resistance test performance required by the flexible printed circuit board. In addition, the invention also provides a hole sealing method.

Description

High-temperature-resistant hole sealing agent and hole sealing method
Technical Field
The invention relates to the field of hole sealing agents, in particular to a high-temperature-resistant hole sealing agent and a hole sealing method.
Background
The flexible printed circuit board is a flexible printed circuit board which is made of polyimide or polyester film as a base material and has high reliability and excellent performance. The flexible printed circuit board or FPC for short has the characteristics of high wiring density, light weight and thin thickness.
For many thermal spray coatings, sealing is a necessary post-treatment process. When the coating is exposed to corrosive and oxidative (sometimes high temperature) environments, sealing is a matter of design consideration. Any thermal spray process, especially flame spraying, deposits a coating that has a porous structure. When the coating is exposed to atmosphere, steam, industrial atmosphere, chemical active substances, corrosive gas and high-temperature environment, corrosive elements are introduced into pores, so that the coating and a substrate are subjected to chemical or electrochemical corrosion, and the coating fails, and in such a case, the coating needs to be sealed. As a post-treatment process of thermal spraying, the main content of the sealing operation is selection of a sealing agent and a construction method.
Therefore, the performance of the sealing agent is particularly important, the traditional sealing agent has poor high-temperature resistance, the property of the traditional sealing agent is easily damaged in a high-temperature environment, in addition, the problems of poor contact resistance and poor weldability are easily caused by adopting raw materials such as chromic acid, cobaltic acid and the like, the environmental protection performance is poor, and the environment and the human body are easily damaged.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a high-temperature-resistant sealant which is free of heavy metal, environment-friendly, degradable, high-temperature-resistant, salt mist-resistant and sweat-resistant and a sealing method.
The purpose of the invention is realized by the following technical scheme:
the high-temperature-resistant sealant comprises the following components in parts by mass:
Figure BDA0001999939110000011
Figure BDA0001999939110000021
in one embodiment, the thickness of the high-temperature-resistant sealant after film formation is 0.8nm to 1.5 nm.
In one embodiment, the pH value of the high-temperature-resistant sealant is 4.0-7.0.
In one embodiment, the film-forming material is at least one of a silicone resin, a furan resin, a phenolic resin, an epoxy resin, an unsaturated polyester, and a silicone ether resin.
In one embodiment, the surfactant is at least one of a hydrocarbon surfactant, a fluorocarbon surfactant, and a biosurfactant.
In one embodiment, the organic solvent is at least one of ethanol, butyl cellosolve, ethylene glycol, propylene glycol, and glycerol.
In one embodiment, the adjuvant is at least one of phytic acid, citric acid, tartaric acid and oleic acid.
The hole sealing method of an embodiment includes the following steps:
carrying out once circulating water washing operation after the flexible circuit board is plated with gold;
under the temperature condition of 40-60 ℃, the flexible circuit board is added into a high-temperature-resistant hole sealing agent for hole sealing operation for 0.5-10 min, and then the hole sealing operation is slowly carried out at a constant speed, wherein the high-temperature-resistant hole sealing agent comprises, by mass, 12-30 parts of octadecanethiol, 1-3 parts of hexadecanethiol, 5-10 parts of polyethylene glycol, 8-12 parts of high-alcohol ethoxylate, 14-28 parts of filler, 3-10 parts of film forming substance, 12-25 parts of surfactant, 1-5 parts of acid-base regulator, 20-50 parts of organic solvent and 5-12 parts of auxiliary agent;
carrying out secondary circulating water washing operation on the flexible circuit board, and then carrying out heat treatment operation at the temperature of 80-90 ℃;
performing salt spray test operation on the flexible circuit board by adopting a sodium chloride solution with the mass percent of 5% at the temperature of 30-40 ℃, wherein the spray pressure is 1.0kg/cm2～1.5kg/cm2The spraying amount is 0.80 ml/h-0.90 ml/h.
In one embodiment, 0.3-0.8 KW of ultrasonic wave is applied simultaneously in the hole sealing operation.
In one embodiment, the salt spray test is performed for 24-72 hours.
The high-temperature-resistant hole sealing agent comprises, by mass, 12-30 parts of octadecanethiol, 1-3 parts of hexadecanethiol and poly (ethylene glycol)5 to 10 parts of glycol, 8 to 12 parts of high alcohol ethoxylate, 14 to 28 parts of filler, 3 to 10 parts of film forming substance, 12 to 25 parts of surfactant, 1 to 5 parts of acid-base regulator, 20 to 50 parts of organic solvent and 5 to 12 parts of auxiliary agent, and does not contain any heavy metal such as chromic acid, cobaltic acid and the like, thereby solving the problem of poor contact resistance and weldability of the flexible circuit board caused by using chromic acid and cobaltic acid in the past, wherein the pressure at the joint is not less than 10g/m m2Under the condition (2), the contact resistance change before and after the high-temperature resistant hole sealing agent treatment is not more than 5% (< 0.05m omega), and the high-frequency performance is as follows: the standing-wave ratio is less than or equal to 1.03, the attenuation is less than or equal to 0.08db, and the separation force is reduced by more than 35% before and after treatment; in addition, the flexible printed circuit board can resist the high temperature of 280 ℃, can be continuously supplemented for use, is harmless to the environment and human bodies, can be degraded automatically, can greatly improve the salt spray resistance and the high temperature resistance of the gold-plated flexible printed circuit board, and particularly can improve the acid sweat resistance test performance required by the flexible printed circuit board.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a flowchart illustrating a method of sealing holes according to an embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The high-temperature-resistant sealant comprises the following components in parts by mass:
Figure BDA0001999939110000041
it should be noted that the hole sealing treatment is mainly to seal and fill microscopic pores on the surface of the product, so as to improve the corrosion resistance of the product. However, the traditional sealing agent for the flexible circuit board can bear lower temperature, and is used in a higher temperature environment, for example, in a thermal spraying environment, the physical and chemical properties of the sealing agent are easily damaged, so that a better sealing effect cannot be obtained, for example, problems of foaming, cracking and the like can occur in some cases, the sealing effect of the flexible circuit board is greatly reduced, and the sealing agent cannot meet the production and use requirements. Therefore, in order to improve the high temperature resistance of the sealing agent, the high temperature resistant sealing agent of the embodiment provides an optimized component formula of the high temperature resistant sealing agent obtained through continuous practical analysis, and the obtained high temperature resistant sealing agent has more excellent high temperature resistance by adopting the components with specific mixture ratio. Specifically, compared with a flexible circuit board which is not processed and has the same thickness, the flexible circuit board processed by the high-temperature-resistant hole sealing agent is remarkably improvedThe corrosion resistance of the flexible circuit board is improved, for example, the flexible circuit board can have excellent discoloration prevention and corrosion prevention effects in corrosion tests of sulfur dioxide, hydrogen sulfide, sodium sulfide, potassium sulfide, natural exposure and the like. Secondly, the flexible circuit board can be in a lubricating and protecting environment, so that adverse effects on the flexible circuit board caused by operation and use and the surrounding environment are avoided or greatly reduced, the reliability of the flexible circuit board is effectively ensured, and the conductivity, the insulativity, the weldability and the high-frequency performance of the flexible circuit board are not influenced; thirdly, the components without any heavy metal such as chromic acid, cobaltic acid and the like are adopted, so that the problem of poor contact resistance and weldability of the flexible circuit board caused by using chromic acid and cobaltic acid in the past is solved, and particularly, the contact pressure is not less than 10g/m m2Under the condition (2), the contact resistance change of the flexible circuit board before and after the high-temperature resistant hole sealing agent treatment is not more than 5% (< 0.05m omega), and the high-frequency performance is as follows: standing wave ratio is less than or equal to 1.03, attenuation is less than or equal to 0.08db, and lubricating performance is as follows: the separation force before and after treatment is reduced by more than 35%, especially the flexible printed circuit board can resist the high temperature of 280 ℃, can be continuously supplemented for use, can be automatically degraded, has no harm to the environment and human bodies, obviously improves the salt spray resistance and the high temperature resistance of the gold-plated flexible printed circuit board, and particularly can improve the acid sweat resistance test performance required by the flexible printed circuit board.
It can be understood that octadecanethiol and hexadecanethiol can make the high temperature-resistant sealant have better high temperature resistance, because in thiol, sulfur atom is in an unequal sp hybridization state, two one-electron occupied sp hybridization orbitals respectively form sigma bonds with hydrocarbon carbon and hydrogen, and two lone-pair electrons occupy the other two sp hybridization orbitals. As the hybridized orbit formed by the 3S and 3p orbits of sulfur is larger than the hybridized orbit formed by the 2S and 2p orbits of oxygen, C-S and S-H bonds are respectively longer than C-O and O-H bonds, and the boiling point of mercaptan is higher than that of alkane with similar molecular weight, octadecanethiol and hexadecanethiol are adopted as one of the main components of the high-temperature-resistant sealant, so that the components of the high-temperature-resistant sealant can be better dissolved and mixed, a better sealing effect can be obtained, and particularly the high-temperature-resistant sealant has higher boiling point and corrosion resistance, and the high-temperature resistance performance is better. PolyethyleneThe glycol is non-toxic and non-irritant, has good water solubility, has good intermiscibility with a plurality of components, can improve the overall dispersity and stability of the high-temperature-resistant sealant, and simultaneously enables the high-temperature-resistant sealant to have better wettability so as to achieve better sealing effect, for example, in one embodiment, the molecular weight of the polyethylene glycol is 200. It is understood that the high alcohol ethoxylate has long chain groups, has the advantages of good stability and high temperature resistance, can better disperse and mix the components in the high temperature resistant sealant, has good wetting dispersibility, and particularly can enable the high temperature resistant sealant to have better high temperature resistance and stability, for example, in one embodiment, the high alcohol ethoxylate is C9-11And for another example, the high alcohol ethoxylate is high-carbon fatty alcohol polyoxyethylene ether or octyl phenol polyoxyethylene ether, so that the wettability and the high-temperature resistance of the high-temperature-resistant sealant can be greatly improved. It is understood that the high temperature resistant sealant can be better prevented from being damaged in the high temperature environment by adopting the high temperature resistant filler, for example, the filler is barium sulfate and/or silicon dioxide. It is further noted that the film-forming material can close the micropores on the surface of the metal coating, greatly reduce the porosity, and reduce the electrochemical corrosion between the metal coating and the substrate metal, for example, in one embodiment, the film-forming material is at least one of silicone resin, furan resin, phenolic resin, epoxy resin, unsaturated polyester, and silicone ether resin. For example, the film-forming material is a silicone resin, which is understood to be a class of low molecular weight thermosetting resins in polyorganosiloxanes. The silicone resin can maintain excellent electrical performance after being used continuously at a high temperature range (200-250 ℃) for a long time, and the Si-O bond of the silicone resin has high bonding energy, so the silicone resin is relatively stable and has high heat resistance and high temperature resistance. Meanwhile, the high-temperature-resistant sealant has good arc resistance and hydrophobic and moisture-proof performance, so that the high-temperature resistance and the stability of the high-temperature-resistant sealant can be greatly improved; as another example, the film-forming material is a furan resin, it being understood that the furan resin is made from furfural orThe condensation polymerization product obtained by homopolymerization of the furfuryl alcohol or copolycondensation of the furfuryl alcohol and other monomers is a thermosetting resin with excellent heat resistance and corrosion resistance, so that the film forming substance is furan resin, and the high-temperature resistance and corrosion resistance of the high-temperature resistant sealant are more excellent; for another example, the film-forming substance is phenolic resin, and it can be understood that the phenolic resin has excellent heat resistance, flame resistance, acid resistance, water resistance and insulating property, and good mechanical and electrical properties, so that the high-temperature-resistant sealant adopts phenolic resin as the film-forming substance, and can better seal micropores on the surface of the metal plating layer of the flexible circuit board, greatly reduce porosity, and reduce electrochemical corrosion between the metal plating layer and the substrate; for another example, the film-forming substance is a mixture of epoxy resin, unsaturated polyester and siloxane resin, three thermosetting resins with excellent performance are compounded to obtain a compound film-forming substance, the excellent performance of each component is fully utilized, and the film-forming substance with better performance is obtained under the synergistic effect, so that the high-temperature-resistant sealant is coated on the flexible circuit board to form a protective film with more stable and thinner performance, the porosity of the flexible circuit board is greatly reduced, the salt mist resistance and the high temperature resistance of the flexible circuit board after gold plating are greatly improved, and particularly the acid-resistant sweat test performance required by the flexible circuit board can be improved.
It can be understood that the addition of the surfactant makes the surface of the coated flexible circuit board more flat and uniform. Particularly, the high-temperature-resistant hole sealing agent obtained by simultaneously adopting octadecanethiol, a film forming substance and a surfactant can obtain a better hole sealing effect. For example, in one embodiment, the surfactant is at least one of a hydrocarbon surfactant, a fluorocarbon surfactant, and a biosurfactant. Therefore, the high-temperature-resistant sealant has better surface performance and better coating and sealing effects; for another example, the surfactant is a hydrocarbon surfactant, and further, the surfactant is a nonionic hydrocarbon surfactant, so that it can be understood that the nonionic hydrocarbon surfactant has the advantages of high surface activity, large micelle aggregation number, strong solubilization and high stability, and thus, by adopting the nonionic hydrocarbon surfactant, components in the high-temperature-resistant sealant can be better dissolved, so that better physicochemical properties can be obtained, and the high-temperature-resistant sealant can achieve a better sealing effect. For another example, the surfactant is a fluorocarbon surfactant, and it can be understood that the fluorocarbon surfactant has the characteristics of high surface activity and good heat resistance stability and chemical stability, so that the wettability of the high-temperature-resistant sealant can be improved, and the heat resistance stability and the chemical stability of the high-temperature-resistant sealant can be improved; as another example, the surfactant is a biosurfactant, and it is understood that the biosurfactant is a degradable surfactant. The biosurfactant not only has the common properties of surfactants such as solubilization, emulsification, wetting, foaming, dispersion and surface tension reduction, but also has the advantages of no toxicity, biodegradability, ecological safety, high surface activity and the like compared with other surfactants produced by a chemical synthesis or petroleum refining method, and can improve the environmental protection property of the high-temperature resistant hole sealing agent. For another example, the biosurfactant is sophorolipid or rhamnolipid. For another example, the surfactant is a compound surfactant of a hydrocarbon surfactant, a fluorocarbon surfactant and a biosurfactant, so that through compounding, the addition and synergism effect is generated among the surfactants, the performance superior to that of a single surfactant can be obtained, the using amount of the surfactant can be reduced, and further, the using cost of the high-temperature-resistant hole sealing agent and the pollution to the environment can be reduced.
In order to obtain better sealing quality, for example, in one embodiment, the pH value of the high-temperature resistant sealing agent is 4.0-7.0. Therefore, by controlling the pH value of the high-temperature-resistant sealant, the deposition amount of gold in the flexible circuit board can be the largest, and a better hole sealing effect is obtained. For another example, the pH value of the high temperature resistant sealant is 6.0, so that the sealing performance of the high temperature resistant sealant is optimal. For another example, in one embodiment, the acid-base modifier is glacial acetic acid or a sodium hydroxide solution, so that the pH value required by the high-temperature-resistant sealant can be obtained more easily, and meanwhile, the glacial acetic acid or the sodium hydroxide solution is lower in cost, which is also beneficial to reducing the production cost.
It can be understood that the organic solvent plays a role of a medium for dispersing the solute, and forms a uniform and stable mixture together with the solute, and after the high-temperature resistant sealant is coated on the surface of the flexible circuit board, the solvent gradually volatilizes to leave the solute, so that a protective film is formed to play a role in sealing and protecting. In one embodiment, the organic solvent is at least one of ethanol, butyl cellosolve, ethylene glycol, propylene glycol, and glycerol. Therefore, the components in the high-temperature-resistant sealant can be better mixed and dissolved, and are dispersed more uniformly, so that better hole sealing performance is obtained. For another example, the organic solvent is a mixed solvent of ethanol, ethylene glycol butyl ether, ethylene glycol, propylene glycol and glycerol, and by adopting the compounded organic solvent, the organic solvent with better dispersion performance and permeability can be obtained, so that other components are better mutually fused, the high-temperature-resistant hole sealing agent with higher stability and better overall performance is formed, and a better hole sealing effect is obtained.
In order to further improve the sealing effect of the high-temperature resistant sealing agent, some additives are also added into the high-temperature resistant sealing agent, for example, in one embodiment, the additives are at least one of phytic acid, citric acid, tartaric acid and oleic acid. For example, the auxiliary agent is phytic acid, and the phytic acid has great chelating potential energy, so that the phytic acid has excellent corrosion resistance, the corrosion resistance of the high-temperature-resistant sealant can be obviously improved, the flexible circuit board can be better protected, and the flexible circuit board can be better filled and sealed. For another example, the assistant is citric acid, and it can be understood that the citric acid or citrate is used as a builder, so that metal ions can be rapidly precipitated, the pollutants are prevented from being attached to the flexible circuit board to form a protective film, and the corrosion problem of the flexible circuit board is prevented; for another example, the auxiliary agent is a mixture of phytic acid, citric acid, tartaric acid and oleic acid, and an acidic solution is added into the formula of the high-temperature-resistant sealant, so that the high-temperature-resistant sealant and the flexible circuit board can be better filled and sealed, a better sealing effect is obtained, and the flexible circuit board can be prevented from being oxidized and corroded.
The high-temperature-resistant hole sealing agent prepared by adopting the components without any heavy metal such as chromic acid, cobaltic acid and the like can greatly reduce the problem that a passivation layer is formed on the surface of the coating of the flexible circuit board due to oxidation, greatly solve the corrosion resistance problem of the coating of the flexible circuit board, and avoid the problems of metal welding failure and the like. Especially, the flexible printed circuit board can resist the high temperature of 280 ℃, can be continuously supplemented for use, is harmless to the environment and human bodies, can be automatically degraded, can greatly improve the salt spray resistance and the high temperature resistance of the gold-plated flexible printed circuit board, and especially can improve the acid sweat resistance test performance required by the flexible printed circuit board. For example, in one embodiment, the thickness of the high-temperature-resistant sealant after film formation is 0.8nm to 1.5nm, so that the flexible printed circuit board is treated by the high-temperature-resistant sealant with a better sealing effect, and the sealant is lighter and thinner while achieving a better filling effect, so that the high-temperature-resistant sealant can be used for the flexible printed circuit board with higher requirements on weight and thickness.
In order to continuously optimize the high temperature resistance and the sealing performance of the high temperature resistant sealing agent, for example, in another embodiment, the high temperature resistant sealing agent comprises the following components, by mass, 15-25 parts of octadecanethiol, 2-3 parts of hexadecanethiol, 7-10 parts of polyethylene glycol, 8-12 parts of high alcohol ethoxylate, 16-25 parts of filler, 4-7 parts of film forming substance, 16-20 parts of surfactant, 2-4 parts of acid-base regulator, 24-40 parts of organic solvent and 7-10 parts of auxiliary agent. Therefore, by adjusting and optimizing the proportion of each component of the high-temperature-resistant sealant, various performances of the high-temperature-resistant sealant can be optimized, and particularly the high-temperature-resistant and sealing performances are remarkably improved. For another example, in another embodiment, the high-temperature-resistant sealant comprises, by mass, 20 parts of octadecanethiol, 2 parts of hexadecanethiol, 8 parts of polyethylene glycol, 10 parts of high-alcohol ethoxylate, 18 parts of filler, 6 parts of a film-forming substance, 18 parts of a surfactant, 3 parts of an acid-base regulator, 30 parts of an organic solvent and 8 parts of an auxiliary agent. Therefore, the formula and the specific proportion of the high-temperature-resistant sealant are further optimized, so that the performance of the high-temperature-resistant sealant is more stable and better, and the sealant is more suitable for sealing operation of a flexible circuit board.
Referring to fig. 1, an embodiment of a hole sealing method includes the following steps:
s100, carrying out once circulating water washing operation after gilding the flexible circuit board.
The gold is applied to the FPC for surface treatment, and a nickel-gold plating layer with stable color, good brightness, smooth plating layer and good weldability can be plated on the surface of the flexible circuit board. Therefore, after the gold plating operation is carried out on the flexible circuit board, the nickel-gold plating layer with stable color, good brightness, smooth plating layer and good weldability can be plated on the surface of the flexible circuit board, so that the flexible circuit board obtains better protection effect. For example, in the present embodiment, the flexible wiring board is gold-plated to a thickness of 0.1 μm to 0.015 μm. After the gold plating operation is finished, one-time circulating water washing operation is carried out, redundant gold in the gold plating operation process can be removed, and the flexible circuit board is favorable for keeping good weldability and ductility. For another example, in order to avoid bringing impurities into the flexible printed circuit board, for example, distilled water is used to perform a circular washing operation on the gold-plated flexible printed circuit board, which is beneficial to obtain a better hole sealing effect subsequently.
S200, adding the flexible circuit board into the high-temperature-resistant hole sealing agent at the temperature of 40-60 ℃ to perform hole sealing operation for 0.5-10 min, and then slowly and uniformly extracting.
The flexible circuit board is added into the high-temperature-resistant hole sealing agent to be subjected to hole sealing operation for 0.5-10 min under the condition that the temperature is controlled to be 40-60 ℃, and microscopic pores on the surface of the flexible circuit board can be sealed and filled to improve the corrosion resistance of the flexible circuit board. It can be understood that under the temperature condition of 40-60 ℃, the high-temperature-resistant hole sealing agent can keep better activity and has better hole sealing effect. In addition, it should be noted that, during the whole process of hole sealing, the workpiece slightly shakes or the solution is stirred, so that the film layer originally wrapped by the water film can be quickly replaced by the hole sealing solution to be soaked, and the possibility of uneven sealing effect is avoided. For example, in one embodiment, 0.3KW to 0.8KW of ultrasonic waves are also applied simultaneously in performing the sealing operation. Therefore, the flexible circuit board is kept in a vibrating state in the hole sealing operation process, the surface of the flexible circuit board can be guaranteed to be soaked, and the hole sealing treatment effect is prevented from being influenced by the hole. After the hole sealing operation is finished, the flexible circuit board is slowly lifted out at a constant speed, so that the damage to the uniformity and stability of a protective film on the flexible circuit board is avoided, and the subsequent further treatment is facilitated.
In order to obtain better sealing effect, for example, the high-temperature-resistant sealing agent comprises, by mass, 12-30 parts of octadecanethiol, 1-3 parts of hexadecanethiol, 5-10 parts of polyethylene glycol, 8-12 parts of high-alcohol ethoxylate, 14-28 parts of filler, 3-10 parts of film-forming substance, 12-25 parts of surfactant, 1-5 parts of acid-base regulator, 20-50 parts of organic solvent and 5-12 parts of auxiliary agent. By adopting the components in a specific ratio, the obtained high-temperature-resistant hole sealing agent has more excellent high-temperature resistance. Specifically, compared with a flexible circuit board which is not processed and has the same thickness, the flexible circuit board processed by the high-temperature-resistant hole sealing agent has the advantages that the corrosion resistance is remarkably improved, and for example, the flexible circuit board has excellent anti-discoloration and anti-corrosion effects in corrosion tests of sulfur dioxide, hydrogen sulfide, sodium sulfide, potassium sulfide, natural exposure and the like. Secondly, the flexible circuit board can be in a lubricating and protecting environment, so that adverse effects on the flexible circuit board caused by operation and use and the surrounding environment are avoided or greatly reduced, the reliability of the flexible circuit board is effectively ensured, and the conductivity, the insulativity, the weldability and the high-frequency performance of the flexible circuit board are not influenced; thirdly, the components without any heavy metal such as chromic acid, cobaltic acid and the like are adopted, so that the problem of poor contact resistance and weldability of the flexible circuit board caused by using chromic acid and cobaltic acid in the past is solved, and particularly, the contact pressure is not less than 10g/m m2Under the condition (2), the contact resistance change of the flexible circuit board before and after the high-temperature resistant hole sealing agent treatment is not more than 5% (< 0.05m omega), and the high-frequency performance is as follows: standing wave ratio is less than or equal to 1.03, attenuation is less than or equal to 0.08db, and lubricating performance is as follows: the separation force before and after treatment is reduced by more than 35%, especially the flexible printed circuit board can resist the high temperature of 280 ℃, can be continuously supplemented for use, can be automatically degraded, has no harm to the environment and human bodies, obviously improves the salt spray resistance and the high temperature resistance of the gold-plated flexible printed circuit board, and particularly can improve the acid sweat resistance test performance required by the flexible printed circuit board. For another example, the high-temperature-resistant hole sealing agent of another embodiment comprises, by mass, 15 to 25 parts of octadecanethiol, 2 to 3 parts of hexadecanethiol, 7 to 10 parts of polyethylene glycol, 9 to 11 parts of high alcohol ethoxylate, 16 to 25 parts of filler, 4 to 7 parts of film-forming substance, 16 to 20 parts of surfactant, 2 to 4 parts of acid-base regulator, 24 to 40 parts of organic solvent and 7 to 10 parts of auxiliary agent. Therefore, by adjusting and optimizing the proportion of each component of the high-temperature-resistant sealant, various performances of the high-temperature-resistant sealant can be optimized, and particularly the high-temperature-resistant and sealing performances are remarkably improved. For another example, the high-temperature-resistant sealant of another embodiment comprises, by mass, 20 parts of octadecanethiol, 2 parts of hexadecanethiol, 8 parts of polyethylene glycol, 10 parts of high alcohol ethoxylate, 18 parts of filler, 6 parts of a film-forming substance, 18 parts of a surfactant, 3 parts of an acid-base regulator, 30 parts of an organic solvent and 8 parts of an auxiliary agent. Therefore, the formula and the specific proportion of the high-temperature-resistant sealant are further optimized, so that the performance of the high-temperature-resistant sealant is more stable and better, and the sealant is more suitable for sealing operation of a flexible circuit board.
S300, performing secondary circulating water washing operation on the flexible circuit board, and performing heat treatment operation at the temperature of 80-90 ℃.
It can be understood that the flexible circuit board is extracted after being soaked in the high-temperature-resistant hole sealing agent for 0.5-10 min, the high-temperature-resistant hole sealing agent still remains on the surface or in the gap, and in order to avoid the influence on the safety of human bodies and the environment, the flexible circuit board is subjected to secondary circulation water washing operation, for example, the time for performing the secondary circulation water washing operation is 15-30 min, so that the residual high-temperature-resistant hole sealing agent on the flexible circuit board can be thoroughly removed, then, the heat treatment operation is performed under the temperature condition of 80-90 ℃, and the water stain on the flexible circuit board is further removed and dried, so that the flexible circuit board with uniform plating layer and better weldability is obtained. It should be especially noted that, in order to avoid the damage of the high temperature resistant sealant caused by the excessively high heat treatment temperature, for example, in one embodiment, the heat treatment operation includes the following steps: s310, preheating the flexible circuit board for 5-8 min at the temperature of 80-85 ℃; s320, drying the flexible circuit board for 12-25 min at the temperature of 86-90 ℃; s330, cooling the flexible circuit board. Therefore, in the beginning stage of heat treatment, the water stain on the flexible circuit board is slowly removed by controlling the lower heat treatment temperature, and meanwhile, the phenomenon that the sealant on the flexible circuit board generates bubbles due to sudden high temperature can be avoided, and particularly, the surface of the flexible circuit board forms a rough surface after the bubbles are broken, so that the qualified rate of products is influenced; and after preheating, carry out the high temperature stoving operation of longer time again, can guarantee fast will water stain on the flexible printed circuit board surface is dried, can guarantee again the homogeneity and the weldability of cladding material on the flexible printed circuit board, after the high temperature stoving operation, for the convenience of follow-up further operation, through right flexible printed circuit board cools down the cooling operation, can avoid scalding operating personnel to guarantee the security of follow-up operation.
S400, performing salt spray test operation on the flexible circuit board by adopting a sodium chloride solution with the mass percent of 5% at the temperature of 30-40 ℃, wherein the spray pressure is 1.0kg/cm2～1.5kg/cm2The spraying amount is 0.80 ml/h-0.90 ml/h.
It is understood that most corrosion occurs in atmospheric environments, which contain corrosive elements and corrosion factors such as oxygen, humidity, temperature changes, and contaminants. Salt spray corrosion is a common and most destructive atmospheric corrosion. The salt fog causes corrosion to the surface of the metal material because the contained chloride ions penetrate through the oxide layer and the protective layer of the metal surface to generate electrochemical reaction with the internal metal. Thus, in order to improve the quality of the flexible circuit board, salt spray test operation is also performed. For example, the salt spray test operation is carried out on the flexible circuit board by adopting a sodium chloride solution with the mass percent of 5% under the temperature condition of 30-40 ℃, wherein the spraying pressure is 1.0kg/cm2～1.5kg/cm2The spraying amount is 0.80 ml/h-0.90 ml/h. For another example, in one embodiment, the time of the salt spray test operation is 24h to 72h, so that the salt spray test can be performed on the flexible circuit board for a certain time, so as to test the corrosion resistance of the flexible circuit board, which is beneficial to obtaining a flexible circuit board with better quality, for example, the flexible circuit board can pass corrosion tests such as sulfur dioxide, hydrogen sulfide, sodium sulfide, potassium sulfide and natural exposure, and meanwhile, the flexible circuit board has excellent discoloration prevention and corrosion prevention effects.
Compared with the prior art, the invention has at least the following advantages:
the high-temperature-resistant hole sealing agent provided by the invention does not contain components of any heavy metal such as chromic acid, cobaltic acid and the like, solves the problem of poor contact resistance and weldability of a flexible circuit board caused by using chromic acid and cobaltic acid in the past, and particularly, the contact pressure is not less than 10g/m m2Under the condition (2), the contact resistance change of the flexible circuit board before and after the high-temperature resistant hole sealing agent treatment is not more than 5% (< 0.05m omega), and the high-frequency performance is as follows: standing wave ratio is less than or equal to 1.03, attenuation is less than or equal to 0.08db, and lubricating performance is as follows: the separation force before and after treatment is reduced by more than 35%, especially the flexible printed circuit board can resist the high temperature of 280 ℃, can be continuously supplemented for use, can be automatically degraded, has no harm to the environment and human bodies, obviously improves the salt spray resistance and the high temperature resistance of the gold-plated flexible printed circuit board, and particularly can improve the acid sweat resistance test performance required by the flexible printed circuit board.
The following is a detailed description of the embodiments.
Example 1
After the flexible circuit board is plated with gold, carrying out primary circulating water washing operation by using distilled water;
under the temperature condition of 40 ℃, adding the flexible circuit board into a high-temperature-resistant hole sealing agent for hole sealing operation for 0.5min, and then slowly extracting the flexible circuit board at a constant speed, wherein the high-temperature-resistant hole sealing agent comprises, by mass, 12kg of octadecanethiol, 1kg of hexadecanethiol, 5kg of polyethylene glycol, 8kg of high-carbon fatty alcohol polyoxyethylene ether, 8kg of barium sulfate, 6kg of silicon dioxide, 3kg of organic silicon resin, 12kg of hydrocarbon surfactant, 1kg of glacial acetic acid, 20kg of ethanol and 5kg of phytic acid;
after the secondary circulating water washing operation is carried out on the flexible circuit board, drying operation is carried out at the temperature of 80 ℃;
under the temperature condition of 30 ℃, a sodium chloride solution with the mass percentage of 5% is adopted to carry out salt spray test operation on the flexible circuit board for 72 hours, wherein the spray pressure is 1.0kg/cm2The amount of spray was 0.80 ml/h.
Example 2
After the flexible circuit board is plated with gold, carrying out primary circulating water washing operation by using distilled water;
under the temperature condition of 45 ℃, adding the flexible circuit board into a high-temperature-resistant hole sealing agent for hole sealing operation for 1.0min, and then slowly extracting the flexible circuit board at a constant speed, wherein the high-temperature-resistant hole sealing agent comprises the following components, by mass, 15kg of octadecanethiol, 2kg of hexadecanethiol, 7kg of polyethylene glycol, 9kg of high-carbon fatty alcohol polyoxyethylene ether, 9kg of barium sulfate, 7kg of silicon dioxide, 5kg of furan resin, 15kg of a hydrocarbon surfactant, 2kg of glacial acetic acid, 25kg of ethylene glycol monobutyl ether and 6kg of phytic acid;
after the secondary circulating water washing operation is carried out on the flexible circuit board, drying operation is carried out at the temperature of 80 ℃;
under the temperature condition of 30 ℃, a sodium chloride solution with the mass percentage of 5% is adopted to carry out salt spray test operation on the flexible circuit board for 72 hours, wherein the spray pressure is 1.0kg/cm2The amount of spray was 0.80 ml/h.
Example 3
After the flexible circuit board is plated with gold, carrying out primary circulating water washing operation by using distilled water;
under the temperature condition of 45 ℃, adding the flexible circuit board into a high-temperature-resistant hole sealing agent for hole sealing operation for 3.0min, and then slowly extracting the flexible circuit board at a constant speed, wherein the high-temperature-resistant hole sealing agent comprises, by mass, 20kg of octadecanethiol, 2kg of hexadecanethiol, 8kg of polyethylene glycol, 9kg of octylphenol polyoxyethylene ether, 11kg of barium sulfate, 7kg of silicon dioxide, 6kg of phenolic resin, 18kg of fluorocarbon surfactant, 3kg of sodium hydroxide solution, 30kg of organic solvent and 8kg of citric acid;
after the secondary circulating water washing operation is carried out on the flexible circuit board, drying operation is carried out at the temperature of 85 ℃;
performing salt spray test operation on the flexible circuit board for 72 hours by adopting a sodium chloride solution with the mass percent of 5% at the temperature of 35 ℃, wherein the spray pressure is 1.2kg/cm2The spraying amount was 0.90 ml/h.
Example 4
After the flexible circuit board is plated with gold, carrying out primary circulating water washing operation by using distilled water;
under the temperature condition of 50 ℃, adding the flexible circuit board into a high-temperature-resistant hole sealing agent for hole sealing operation for 5.0min, and then slowly extracting the flexible circuit board at a constant speed, wherein the high-temperature-resistant hole sealing agent comprises, by mass, 28kg of octadecanethiol, 2kg of hexadecanethiol, 9kg of polyethylene glycol, 11kg of octylphenol polyoxyethylene ether, 8kg of phenolic resin, 20kg of a biological surfactant, 4kg of a sodium hydroxide solution, 40kg of ethylene glycol and 10kg of tartaric acid;
after the secondary circulating water washing operation is carried out on the flexible circuit board, drying operation is carried out at the temperature of 85 ℃;
performing salt spray test operation on the flexible circuit board for 72 hours by adopting a sodium chloride solution with the mass percent of 5% at the temperature of 40 ℃, wherein the spray pressure is 1.2kg/cm2The spraying amount was 0.90 ml/h.
Example 5
After the flexible circuit board is plated with gold, carrying out primary circulating water washing operation by using distilled water;
under the temperature condition of 60 ℃, adding the flexible circuit board into a high-temperature-resistant hole sealing agent for hole sealing operation for 3.0min, and then slowly extracting the flexible circuit board at a constant speed, wherein the high-temperature-resistant hole sealing agent comprises, by mass, 30kg of octadecanethiol, 3kg of hexadecanethiol, 10kg of polyethylene glycol, 12kg of octylphenol polyoxyethylene ether, 15kg of barium sulfate, 13kg of silicon dioxide, 3kg of epoxy resin, 3kg of unsaturated polyester, 4kg of silicon ether resin, 25kg of a biosurfactant, 5kg of a sodium hydroxide solution, 15kg of ethylene glycol, 15kg of propylene glycol, 20kg of glycerol, 5kg of tartaric acid and 7kg of oleic acid;
after the secondary circulating water washing operation is carried out on the flexible circuit board, drying operation is carried out at the temperature of 85 ℃;
performing salt spray test operation on the flexible circuit board for 72 hours by adopting a sodium chloride solution with the mass percent of 5% at the temperature of 40 ℃, wherein the spray pressure is 1.2kg/cm2The spraying amount was 0.90 ml/h.
By performing the salt spray test on the flexible circuit board of each embodiment, the indexes are as shown in the following table 1:
TABLE 1
Figure BDA0001999939110000151
In addition, by testing the flexible wiring boards after sealing of examples 1 to 5, the contact pressure was not less than 10g/m m2Under the condition (2), the contact resistance change of the flexible circuit board before and after the high-temperature resistant hole sealing agent treatment is not more than 5% (< 0.05m omega), and the high-frequency performance is as follows: the standing-wave ratio is less than or equal to 1.03, the attenuation is less than or equal to 0.08db, and the separation force is reduced by more than 35% before and after treatment; in addition, under the high temperature condition of 280 ℃, the high temperature resistant sealant at the sealing hole still has no problem of bubbles or cracks, and the applicability of the high temperature environment is obviously improved.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (9)

1. The high-temperature-resistant hole sealing agent is characterized by comprising the following components in parts by mass:
Figure FDA0002889313160000011
the film forming substance is at least one of organic silicon resin, furan resin, phenolic resin, epoxy resin, unsaturated polyester and silicon ether resin;
the high alcohol ethoxylate is high-carbon fatty alcohol polyoxyethylene ether or octyl phenol polyoxyethylene ether.
2. The high-temperature-resistant sealant according to claim 1, wherein the thickness of the high-temperature-resistant sealant after film formation is 0.8nm to 1.5 nm.
3. The high-temperature-resistant sealant according to claim 1, wherein the pH value of the high-temperature-resistant sealant is 4.0-7.0.
4. The high temperature resistant sealant according to claim 1, wherein the surfactant is at least one of a hydrocarbon surfactant, a fluorocarbon surfactant and a biosurfactant.
5. The high temperature resistant sealant according to claim 1, wherein the organic solvent is at least one of ethanol, butyl cellosolve, ethylene glycol, propylene glycol and glycerol.
6. The high temperature resistant sealant according to claim 1, wherein the auxiliary agent is at least one of phytic acid, citric acid, tartaric acid and oleic acid.
7. The hole sealing method is characterized by comprising the following steps:
carrying out once circulating water washing operation after the flexible circuit board is plated with gold;
under the temperature condition of 40-60 ℃, the flexible circuit board is added into a high-temperature-resistant hole sealing agent for hole sealing operation for 0.5-10 min, and then the hole sealing operation is slowly carried out at a constant speed, wherein the high-temperature-resistant hole sealing agent comprises, by mass, 12-30 parts of octadecanethiol, 1-3 parts of hexadecanethiol, 5-10 parts of polyethylene glycol, 8-12 parts of high-alcohol ethoxylate, 14-28 parts of filler, 3-10 parts of film forming substance, 12-25 parts of surfactant, 1-5 parts of acid-base regulator, 20-50 parts of organic solvent and 5-12 parts of auxiliary agent;
carrying out secondary circulating water washing operation on the flexible circuit board, and then carrying out heat treatment operation at the temperature of 80-90 ℃;
performing salt spray test operation on the flexible circuit board by adopting a sodium chloride solution with the mass percent of 5% at the temperature of 30-40 ℃, wherein the spray pressure is 1.0kg/cm2～1.5kg/cm2The spraying amount is 0.80 ml/h-0.90 ml/h.
8. The method according to claim 7, wherein 0.3KW to 0.8KW of ultrasonic waves are also applied simultaneously in performing the hole sealing operation.
9. The hole sealing method according to claim 7, wherein the time of the salt spray test operation is 24-72 h.
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