CN116145226A - Stripping solution for PCB (printed circuit board) manufacturing process and application method thereof - Google Patents
Stripping solution for PCB (printed circuit board) manufacturing process and application method thereof Download PDFInfo
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- CN116145226A CN116145226A CN202310176800.8A CN202310176800A CN116145226A CN 116145226 A CN116145226 A CN 116145226A CN 202310176800 A CN202310176800 A CN 202310176800A CN 116145226 A CN116145226 A CN 116145226A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25F—PROCESSES FOR THE ELECTROLYTIC REMOVAL OF MATERIALS FROM OBJECTS; APPARATUS THEREFOR
- C25F5/00—Electrolytic stripping of metallic layers or coatings
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
- H05K3/06—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding the conductive material being removed chemically or electrolytically, e.g. by photo-etch process
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/02—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding
- H05K3/06—Apparatus or processes for manufacturing printed circuits in which the conductive material is applied to the surface of the insulating support and is thereafter removed from such areas of the surface which are not intended for current conducting or shielding the conductive material being removed chemically or electrolytically, e.g. by photo-etch process
- H05K3/061—Etching masks
- H05K3/062—Etching masks consisting of metals or alloys or metallic inorganic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention provides a stripping solution for PCB (printed circuit board) process technology, which comprises raw materials including an oxidant, a composite complexing agent, a corrosion inhibitor, a penetrating agent, a buffering agent, an auxiliary agent and water; the composite material with extremely strong complexing capability is selected, so that a large amount of chelate adsorption deplating metal can be realized, the service life of the deplating liquid is greatly prolonged, and the subsequent deplating metal regeneration and recovery are facilitated; the traditional corrosion inhibitor after activation and modification can greatly improve the activity of core corrosion inhibition components in low-temperature stripping liquid, and improve the protective force on a workpiece substrate; the mixture of the linoleoyl diethanolamine and the soyanoyl diethanolamine with strong dispersion capability is used as the strengthening modifier, so that on one hand, the permeability of sodium alkylbenzenesulfonate and sulfonated oil can be greatly improved, and meanwhile, the stripping strength of stripping solution to a coating is enhanced, and the stripping uniformity is improved.
Description
Technical Field
The invention belongs to the technical field of PCB manufacture, and particularly relates to a stripping solution for a PCB manufacturing process and a use method thereof.
Background
A printed circuit board, abbreviated as PCB, is an essential core component of an electronic product. Along with the development trend of integration, high density and high reliability of electronic products, the design of the PCB is more compact, light, thin, short, multifunctional and intelligent, and the quality requirement on the PCB is higher.
In the PCB manufacturing process, in order to protect the conductive area from etching damage, a corrosion-resistant metal layer is plated on the conductive area, and the metal plating layer is removed by using a stripping solution after the etching process. However, there are many problems in the industry that affect the process efficiency, yield, and environment when using the stripping solution, such as: 1. the stripping rate is difficult to control, the stripping effect is poor, and the phenomenon of corrosion of a protected conductive area or incomplete stripping is easy to occur; 2. the deplating process generates a large amount of toxic and harmful gas, which affects the physical and psychological health of operators and has high environmental protection pressure; 3. the stripping operation temperature is high, and the energy waste is serious.
Based on the above problems, the application provides a stripping solution for a PCB (printed circuit board) process and a use method thereof, so as to meet the process requirements, improve the process efficiency and yield of the PCB, and reduce the environmental protection risk.
Disclosure of Invention
The first object of the present invention is: a composite complexing agent for use in a stripping solution for PCB processing is provided.
The second object of the present invention is to: a corrosion inhibitor for use in a stripping solution for PCB manufacturing processes is provided.
Another object of the invention is that: a penetrant for use in a stripping solution for PCB manufacturing processes is provided.
A fourth object of the present invention is to: a method for using a stripping solution for PCB manufacturing process is provided.
The invention is realized by the following technical scheme:
the deplating liquid for PCB manufacture process comprises oxidant 150-200g/L, compound complexing agent 15-25g/L, corrosion inhibitor 2-7g/L, penetrating agent 1-2g/L, buffering agent 40-70g/L, auxiliary agent 2-6g/L, water constant volume to 1L; the configuration method comprises the following steps: sequentially dissolving oxidant, compound complexing agent, corrosion inhibitor, penetrating agent and auxiliary agent in water, stirring for 5-15min, adding water to constant volume to 1L, continuously adding buffer, controlling pH to 3.5-5, continuously stirring for 10-20min, and slowly heating to 20-35deg.C.
The oxidant is ammonium nitrate;
the buffering agent is a mixture of sodium acetate and nitrilotriacetic acid with the mass ratio of 3-5:1;
the auxiliary agent is a mixture of sodium chloride and sodium phosphate with the mass ratio of 5-9:1;
the composite complexing agent is prepared from the following components in percentage by mass: 2-6:1, ethylenediamine tetra (sodium methylene phosphate), diethylenetriamine penta (methylene phosphonic acid) sodium and polyhydroxyacrylic acid are taken as main materials, porous materials are taken as carriers, and a composite material with extremely strong complexing ability is formed, and the preparation method specifically comprises the following steps:
(1) Weighing 10-20 parts of main materials according to the mass ratio, ball milling for 20-30min, adding into 50-100 times of water, and uniformly stirring;
(2) Adding 10 times of porous material in weight parts of main material, performing ultrasonic dispersion for 1-2h at 15-25KHz frequency, and standing for adsorption for 24h;
(3) Centrifuging at 50-100rpm for 20-30min, standing for 5min, switching to 500-1000rpm for 10-15min, standing for 20min, switching to 2000-3000rpm for 3-5min, centrifuging, removing supernatant, and oven drying precipitate at 30-50deg.C;
the porous material is one or a mixture of multiple kinds of biochar, molecular sieve and diatomite.
The preparation method of the corrosion inhibitor comprises the following raw materials, by weight, 3-9 parts of a colored benzothiazole, 3-7 parts of a benzotriazole, 5-15 parts of a methylbenzotriazole, 1-3 parts of an activation modifier and 20-30 parts of an ethanol solution, wherein the raw materials comprise the following specific components:
(1) Mixing the azyl benzothiazole, the benzotriazole and the methylbenzotriazole, and grinding and refining for 15-25min to obtain a grinding mixture;
(2) Adding the grinding mixture into ethanol solution, stirring and dispersing at 200-400rpm for 30min, and dispersing the solution;
(3) Adding an activation modifier into the dispersion liquid while stirring, slowly heating to 50 ℃, and continuously stirring for 20-40min to obtain the modified polyurethane foam;
the mass ratio of the activation modifier is 2-6: 1-butyl-2-methylimidazole, a mixture of biological enzymes; the biological enzyme is a mixture of lignin enzyme, pectase and lysozyme in a mass ratio of 1:1:1;
the mass fraction of the ethanol solution is 30-60%.
The preparation method of the penetrating agent comprises the following raw materials, by weight, 15-20 parts of sodium alkylbenzenesulfonate, 5-8 parts of sulfonated oil and 15-30 parts of strengthening modifier, wherein the raw materials comprise the following concrete steps:
(1) Mixing sodium alkylbenzenesulfonate with sulfonated oil, and uniformly stirring;
(2) Adding reinforcing modifier, stirring and dispersing for 30min, stopping stirring, introducing N2, controlling air flow at 200-400mL/min, performing ultrasonic dispersion at 20-30KHz, and stopping ventilation after 2 hr.
The strengthening modifier is a mixture of linoleoyl diethanolamine and soyate diethanolamine with the mass ratio of 1:1-3.
The invention also provides a use method of the stripping solution for the PCB manufacturing process, which comprises the following steps:
(1) Soaking the deplating piece in water at 40-60deg.C for 3-5min;
(2) Taking out, transferring to a deplating solution with the temperature of 20-35 ℃, electrifying and electrolyzing at the voltage of 6-12V for 1-4min;
(3) Taking out, ultrasonic cleaning with water, and oven drying at 30-40deg.C.
The invention has the advantages that:
1. the method is characterized in that the mixture of ethylenediamine tetra (sodium methylene phosphate), diethylenetriamine penta (sodium methylene phosphonate) and polyhydroxyacrylic acid is selected as a main material, a porous material is used as a carrier, a composite material with extremely strong complexing ability is formed through a multistage centrifugal adsorption process, when a workpiece is subjected to deplating, the main complexing agent material loaded on the surface and the inside of the porous material can be chelated and adsorbed in a large amount to deplating metal, the service life of the deplating liquid is greatly prolonged, and meanwhile, the regeneration and recovery of the subsequent deplating metal are facilitated.
2. The core corrosion inhibition component is composed of the azyl benzothiazole, the benzotriazole and the methyl benzotriazole, and the activation modifier is composed of the mixture of the 1-butyl-2-methylimidazole and the biological enzyme, so that the activity of the core corrosion inhibition component in the low-temperature stripping solution can be greatly improved, and the protection force on the workpiece base material is improved.
3. After the composite complexing agent and the activated modified corrosion inhibitor are introduced into the stripping solution, the stripping efficiency and the service life of the stripping solution are greatly improved, and the corrosion to the surface of the PCB substrate is correspondingly reduced a lot, however, the inventor finds that the use of the composite complexing agent and the activated modified corrosion inhibitor can greatly reduce the uniformity of the stripping speed of the stripping workpiece compared with the traditional stripping solution, especially for the part of the PCB workpiece with poor uniformity of the plating layer, the surface of the stripping surface is colored, the plating layer is remained, and the stripping uniformity of the stripping solution is improved compared with the part of the PCB workpiece with poor uniformity of the plating layer, but the stripping surface is still not satisfactory under the low-temperature stripping environment of the invention.
In order to make the stripping solution for PCB manufacturing process more clear, the invention is further described below with reference to the specific embodiments.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
Example 1
A stripping solution for PCB manufacturing process,
1. preparing a composite complexing agent
(1) Weighing the following materials in mass ratio of 5:4:1, 15 parts of main material mixture of ethylenediamine tetra (sodium methylene phosphate), diethylenetriamine penta (methylene phosphonic acid) sodium and polyhydroxyacrylic acid, ball milling for 25min, adding into 80 times of water by mass, and uniformly stirring;
(2) Adding 10 times of biochar in the mass part of the main material mixture, performing ultrasonic dispersion for 1.5 hours at 20KHz frequency, and then standing for adsorption for 24 hours;
(3) Centrifuging at 80rpm for 25min, standing for 5min, switching to 750rpm for 13min, standing for 20min, switching to 2500rpm for 4min, removing supernatant after centrifuging, and oven drying precipitate at 40deg.C to obtain the final product;
2. preparation of corrosion inhibitor
(1) Mixing 6 parts of the azyl benzothiazole, 5 parts of the benzotriazole and 10 parts of the methylbenzotriazole, and grinding and refining for 20 minutes to obtain a grinding mixture;
(2) Adding the grinding mixture into 25 parts of 45% ethanol solution, stirring and dispersing for 30min at a speed of 300rpm, and dispersing liquid;
(3) Adding 2 parts by mass of 4 to the dispersion liquid while stirring: and (3) slowly heating the mixture of 1-butyl-2-methylimidazole, lignin enzyme, pectase and lysozyme to 50 ℃ in a ratio of 1:1:1, and continuously stirring for 30min to obtain the microbial inoculum.
3. Preparation of penetrant
(1) Mixing 18 parts of sodium alkylbenzenesulfonate with 7 parts of sulfonated oil, and uniformly stirring;
(2) Adding 25 parts of a mixture of linoleoyl diethanolamine and soyanoyl diethanolamine with the mass ratio of 1:2 as a strengthening modifier, stirring and dispersing for 30min, stopping stirring, and introducing N 2 Controlling the air flow to be 300mL/min, performing ultrasonic dispersion at 25KHz, and stopping ventilation after 2 hours.
4. Stripping solution for preparing PCB process
180g/L of ammonium nitrate, 20g/L of complexing agent, 5g/L of corrosion inhibitor, 1.5g/L of penetrating agent, 55g/L of mixture of nitrilotriacetic acid with the mass ratio of 4:1, 4g/L of mixture of sodium chloride and sodium phosphate with the mass ratio of 7:1 and water to fix the volume to 1L; sequentially dissolving an oxidant, a composite complexing agent, a corrosion inhibitor, a penetrating agent and an auxiliary agent in water, stirring for 10min, adding water to a constant volume of 1L, continuously adding a buffering agent, controlling the pH value to be 4, and continuously stirring for 15min to obtain the stripping solution.
Example 2
A stripping solution for PCB manufacturing process,
1. preparing a composite complexing agent
(1) Weighing the following components in percentage by mass: 2:1, 20 parts of main material mixture of ethylenediamine tetra (sodium methylene phosphate), diethylenetriamine penta (methylene phosphonic acid) sodium and polyhydroxyacrylic acid, ball milling for 20min, adding into 50 times of water by mass, and uniformly stirring;
(2) Adding 10 times of molecular sieve in the mass part of the main material mixture, performing ultrasonic dispersion for 1h at 25KHz frequency, and then standing for adsorption for 24h;
(3) Centrifuging at 50rpm for 30min, standing for 5min, switching to 500rpm for 10min, standing for 20min, switching to 3000rpm for 3min, removing supernatant after centrifuging, and oven drying precipitate at 30deg.C to obtain the final product;
2. preparation of corrosion inhibitor
(1) Mixing 3 parts of the azyl benzothiazole, 3 parts of the benzotriazole and 15 parts of the methylbenzotriazole, and grinding and refining for 15 minutes to obtain a grinding mixture;
(2) Adding the grinding mixture into 20 parts of ethanol solution with the mass fraction of 60%, stirring and dispersing for 30min at a rotating speed of 200rpm, and dispersing liquid;
(3) Adding 1 part by mass of a mixture into the dispersion liquid while stirring, wherein the mass ratio is 6: and (3) slowly heating the mixture of 1-butyl-2-methylimidazole, lignin enzyme, pectase and lysozyme to 50 ℃ in a ratio of 1:1:1, and continuously stirring for 40min to obtain the microbial inoculum.
3. Preparation of penetrant
(1) Mixing 15 parts of sodium alkylbenzenesulfonate with 5 parts of sulfonated oil, and uniformly stirring;
(2) Adding 30 parts of a mixture of linoleoyl diethanolamine and soyanoyl diethanolamine with the mass ratio of 1:1 as a strengthening modifier, stirring and dispersing for 30min, stopping stirring, and introducing N 2 Controlling the air flow to be 200mL/min, performing ultrasonic dispersion at 30KHz, and stopping ventilation after 2 hours.
4. Stripping solution for preparing PCB process
According to the proportion, 150g/L of ammonium nitrate, 15g/L of complexing agent, 7g/L of corrosion inhibitor, 1g/L of penetrating agent, 40g/L of mixture of nitrilotriacetic acid and sodium chloride with the mass ratio of 5:1, 6g/L of mixture of sodium phosphate and water are fixed to 1L; sequentially dissolving an oxidant, a composite complexing agent, a corrosion inhibitor, a penetrating agent and an auxiliary agent in water, stirring for 5min, adding water to a constant volume of 1L, continuously adding a buffering agent, controlling the pH value to be 3.5, and continuously stirring for 20min to obtain the stripping solution.
Example 3
A stripping solution for PCB manufacturing process,
1. preparing a composite complexing agent
(1) Weighing the following components in percentage by mass: 6:1, 10 parts of main material mixture of ethylenediamine tetra (sodium methylene phosphate), diethylenetriamine penta (methylene phosphonic acid) sodium and polyhydroxyacrylic acid, ball milling for 30min, adding into 100 times of water by mass, and uniformly stirring;
(2) Adding 10 times of diatomite in the mass part of the main material mixture, performing ultrasonic dispersion for 2 hours at the frequency of 15KHz, and then standing for adsorption for 24 hours;
(3) Centrifuging at 100rpm for 20min, standing for 5min, switching to 1000rpm for 15min, standing for 20min, switching to 2000rpm for 5min, removing supernatant after centrifuging, and oven drying precipitate at 50deg.C to obtain the final product;
2. preparation of corrosion inhibitor
(1) Mixing 9 parts of the azyl benzothiazole, 7 parts of the benzotriazole and 5 parts of the methyl benzotriazole, and grinding and refining for 25 minutes to obtain a grinding mixture;
(2) Adding the grinding mixture into 30 parts of ethanol solution with the mass fraction of 30%, stirring and dispersing for 30min at 400rpm, and dispersing liquid;
(3) Adding 3 parts by mass of 2 to the dispersion liquid while stirring: and (3) slowly heating the mixture of 1-butyl-2-methylimidazole, lignin enzyme, pectase and lysozyme to 50 ℃ in a ratio of 1:1:1, and continuously stirring for 20min to obtain the microbial inoculum.
3. Preparation of penetrant
(1) Mixing 20 parts of sodium alkylbenzenesulfonate with 8 parts of sulfonated oil, and uniformly stirring;
(2) 15 parts of a mixture of linoleoyl diethanolamine and soyanoyl diethanolamine with the mass ratio of 1:3 is added as a strengthening modifier, stirred and dispersed for 30min, then stirring is stopped, and N is introduced 2 Controlling the air flow at 400mL/min, performing ultrasonic dispersion at 20KHz, and stopping ventilation after 2 hours.
4. Stripping solution for preparing PCB process
200g/L of ammonium nitrate, 25g/L of complexing agent, 2g/L of corrosion inhibitor, 2g/L of penetrating agent, 70g/L of mixture of nitrilotriacetic acid and sodium chloride with the mass ratio of 9:1, 2g/L of mixture of sodium phosphate and water to 1L; sequentially dissolving an oxidant, a composite complexing agent, a corrosion inhibitor, a penetrating agent and an auxiliary agent in water, stirring for 15min, adding water to a constant volume of 1L, continuously adding a buffering agent, controlling the pH value to be 5, and continuously stirring for 10min to prepare the stripping solution.
Example 4
The stripping solution for the PCB manufacturing process comprises 180g/L of oxidant, 10g/L of composite complexing agent, 5g/L of corrosion inhibitor, 1.5g/L of penetrating agent, 55g/L of buffering agent, 4g/L of auxiliary agent and water to a constant volume of 1L according to the proportion; sequentially dissolving an oxidant, a composite complexing agent, a corrosion inhibitor, a penetrating agent and an auxiliary agent in water, stirring for 10min, adding water to a constant volume of 1L, continuously adding a buffering agent, controlling the pH value to be 4, and continuously stirring for 15min to obtain the stripping solution.
The procedure is as in example 1.
Example 5
The stripping solution for the PCB manufacturing process comprises 180g/L of oxidant, 30g/L of composite complexing agent, 5g/L of corrosion inhibitor, 1.5g/L of penetrating agent, 55g/L of buffering agent, 4g/L of auxiliary agent and water to a constant volume of 1L according to the proportion; sequentially dissolving an oxidant, a composite complexing agent, a corrosion inhibitor, a penetrating agent and an auxiliary agent in water, stirring for 10min, adding water to a constant volume of 1L, continuously adding a buffering agent, controlling the pH value to be 4, and continuously stirring for 15min to obtain the stripping solution.
The procedure is as in example 1.
Example 6
The stripping solution for the PCB manufacturing process comprises the following preparation steps of:
(1) Weighing the following materials in mass ratio of 5:4:1, 15 parts of main material mixture of ethylenediamine tetra (sodium methylene phosphate), diethylenetriamine penta (methylene phosphonic acid) sodium and polyhydroxyacrylic acid, ball milling for 25min, adding into 80 times of water by mass, and uniformly stirring;
(2) Adding 10 times of biochar in the mass part of the main material mixture, performing ultrasonic dispersion for 1.5 hours at 20KHz frequency, and then standing for adsorption for 24 hours;
(3) Centrifuging at 2500rpm for 4min, removing supernatant after centrifuging, and oven drying precipitate at 40deg.C to obtain the final product;
the procedure is as in example 1.
Example 7
The stripping solution for the PCB manufacturing process comprises the following components in percentage by mass: 4:1, a mixture of sodium ethylenediamine tetramethylene phosphate, sodium diethylenetriamine pentamethylene phosphonate, and polyhydroxyacrylic acid;
the procedure is as in example 1.
Example 8
The stripping solution for the PCB manufacturing process comprises 180g/L of oxidant, 20g/L of composite complexing agent, 1g/L of corrosion inhibitor, 1.5g/L of penetrating agent, 55g/L of buffering agent, 4g/L of auxiliary agent and water to a constant volume of 1L according to the proportion; sequentially dissolving an oxidant, a composite complexing agent, a corrosion inhibitor, a penetrating agent and an auxiliary agent in water, stirring for 10min, adding water to a constant volume of 1L, continuously adding a buffering agent, controlling the pH value to be 4, and continuously stirring for 15min to obtain the stripping solution.
The procedure is as in example 1.
Example 9
The stripping solution for the PCB manufacturing process comprises 180g/L of oxidant, 20g/L of composite complexing agent, 10g/L of corrosion inhibitor, 1.5g/L of penetrating agent, 55g/L of buffering agent, 4g/L of auxiliary agent and water to a constant volume of 1L according to the proportion; sequentially dissolving an oxidant, a composite complexing agent, a corrosion inhibitor, a penetrating agent and an auxiliary agent in water, stirring for 10min, adding water to a constant volume of 1L, continuously adding a buffering agent, controlling the pH value to be 4, and continuously stirring for 15min to obtain the stripping solution.
The procedure is as in example 1.
Example 10
A stripping solution for PCB manufacturing process, wherein the preparation method of the corrosion inhibitor is as follows,
(1) Mixing 6 parts of the azyl benzothiazole, 5 parts of the benzotriazole and 10 parts of the methylbenzotriazole, and grinding and refining for 20 minutes to obtain a grinding mixture;
(2) Adding the grinding mixture into 25 parts of 45% ethanol solution, stirring and dispersing for 30min at a speed of 300rpm, and dispersing liquid;
(3) Adding 0.5 part by mass of the mixture into the dispersion liquid while stirring, wherein the mass ratio is 4: 1-butyl-2-methylimidazole and biological enzyme, slowly heating to 50deg.C, and stirring for 30 min;
the procedure is as in example 1.
Example 11
A stripping solution for PCB manufacturing process, wherein the preparation method of the corrosion inhibitor is as follows,
(1) Mixing 6 parts of the azyl benzothiazole, 5 parts of the benzotriazole and 10 parts of the methylbenzotriazole, and grinding and refining for 20 minutes to obtain a grinding mixture;
(2) Adding the grinding mixture into 25 parts of 45% ethanol solution, stirring and dispersing for 30min at a speed of 300rpm, and dispersing liquid;
(3) Adding 2 parts of 1-butyl-2-methylimidazole into the dispersion liquid while stirring, slowly heating to 50 ℃, and continuously stirring for 30min to obtain the preparation;
the procedure is as in example 1.
Example 12
A stripping solution for PCB manufacturing process, wherein the preparation method of the corrosion inhibitor is as follows,
(1) Mixing 6 parts of the azyl benzothiazole, 5 parts of the benzotriazole and 10 parts of the methylbenzotriazole, and grinding and refining for 20 minutes to obtain a grinding mixture;
(2) Adding the grinding mixture into 25 parts of 45% ethanol solution, stirring and dispersing for 30min at 300rpm, and continuing stirring for 30min to obtain the final product;
the procedure is as in example 1.
Example 13
The stripping solution for the PCB manufacturing process comprises 180g/L of oxidant, 20g/L of complexing agent, 5g/L of corrosion inhibitor, 0.5g/L of penetrating agent, 55g/L of buffering agent, 4g/L of auxiliary agent and water to a constant volume of 1L according to the proportion; sequentially dissolving an oxidant, a composite complexing agent, a corrosion inhibitor, a penetrating agent and an auxiliary agent in water, stirring for 10min, adding water to a constant volume of 1L, continuously adding a buffering agent, controlling the pH value to be 4, and continuously stirring for 15min to obtain the stripping solution.
The procedure is as in example 1.
Example 14
The stripping solution for the PCB manufacturing process comprises 180g/L of oxidant, 20g/L of complexing agent, 5g/L of corrosion inhibitor, 3g/L of penetrating agent, 55g/L of buffering agent, 4g/L of auxiliary agent and 1L of water in proportion; sequentially dissolving an oxidant, a composite complexing agent, a corrosion inhibitor, a penetrating agent and an auxiliary agent in water, stirring for 10min, adding water to a constant volume of 1L, continuously adding a buffering agent, controlling the pH value to be 4, and continuously stirring for 15min to obtain the stripping solution.
The procedure is as in example 1.
Example 15
A deplating liquid for PCB manufacture process, wherein the penetrating agent is prepared by the following steps,
(1) Mixing 18 parts of sodium alkylbenzenesulfonate with 7 parts of sulfonated oil, and uniformly stirring;
(2) Adding 10 parts of a mixture of linoleoyl diethanolamine and soyanoyl diethanolamine with the mass ratio of 1:2 as a strengthening modifier, stirring and dispersing for 30min, stopping stirring, and introducing N 2 Controlling the air flow to be 300mL/min, performing ultrasonic dispersion at 25KHz, and stopping ventilation after 2 hours.
The procedure is as in example 1.
Example 16
A deplating liquid for PCB manufacture process, wherein the penetrating agent is prepared by the following steps,
(1) Mixing 18 parts of sodium alkylbenzenesulfonate with 7 parts of sulfonated oil, and uniformly stirring;
(2) Adding 35 parts of a mixture of linoleoyl diethanolamine and soyanoyl diethanolamine with the mass ratio of 1:2 as a strengthening modifier, stirring and dispersing for 30min, stopping stirring, and introducing N 2 Controlling the air flow to be 300mL/min, performing ultrasonic dispersion at 25KHz, and stopping ventilation after 2 hours.
The procedure is as in example 1.
Example 17
A stripping solution for PCB manufacturing process, wherein the penetrating agent is a mixture of 18 parts by weight of sodium alkylbenzenesulfonate and 7 parts by weight of sulfonated oil.
The procedure is as in example 1.
Test
Test 1
The stripping efficiency, copper corrosion, service life of the stripping solution and surface condition of the PCB copper plate after stripping are measured by the stripping solution prepared in each embodiment, and the method comprises the following steps:
(1) Marking the stripping solutions prepared in the above examples 1-17 as No. 1 stripping solution-No. 17 stripping solution, respectively, and heating to 25deg.C for use;
(2) Taking 170 PCB nickel plating plates which are required to be deplated in the same batch, wherein the nickel plating layers are 6um, randomly and averagely dividing into 17 groups, namely a No. 1 sample group-a No. 17 sample group, soaking in water at 50 ℃ for 4min, and taking out;
(3) And (3) respectively placing the PCB nickel plating plates into No. 1 stripping liquid-No. 17 stripping liquid according to the number, starting stripping, recording the stripping state during the process, visually measuring the time after the plating layer is stripped, respectively taking out and cleaning with water, and testing the residual thickness of each tested PCB nickel plating plate.
Wherein:
nickel stripping rate= (initial nickel layer thickness-nickel layer thickness after stripping end)/nickel stripping time is the average value in the group;
copper corrosion rate = copper corrosion thickness/nickel withdrawal time, as the average value within the group;
the results are calculated and summarized in the following table:
from the above table results it can be seen that:
(1) The test results of the stripping solution samples of each example are better with the results of examples 1-3, especially with the results of example 1;
(2) Compared with examples 1 and 4-7, the addition amount of the composite complexing agent in examples 4 and 5 is too small or too large, the centrifugal mode of the composite complexing agent in example 6 does not meet the technical requirements when the composite complexing agent is prepared, the composite complexing agent in example 7 is not combined with biochar in a bearing way, and the nickel removal rate and the copper corrosion effect are not as good as those of example 1 implemented by adopting the technical scheme of the invention;
(3) The correct choice and use of corrosion inhibitors has a great influence on the protection of the PCB copper substrate during deplating, as can be seen from the comparison of examples 8-12 with example 1;
(4) In order to ensure that the surface of the PCB copper substrate after deplating is uniform and bright, no plating layer is remained, the result of the embodiment 1 implemented by adopting the penetrating agent in the technical scheme of the invention is obviously better than the results of the embodiments 13-17.
Claims (7)
1. A stripping solution for PCB manufacturing process is characterized in that: the raw materials comprise 150-200g/L of oxidant, 15-25g/L of compound complexing agent, 2-7g/L of corrosion inhibitor, 1-2g/L of penetrating agent, 40-70g/L of buffering agent, 2-6g/L of auxiliary agent and water with constant volume to 1L;
the oxidant is ammonium nitrate;
the buffering agent is a mixture of sodium acetate and nitrilotriacetic acid with the mass ratio of 3-5:1;
the auxiliary agent is a mixture of sodium chloride and sodium phosphate with the mass ratio of 5-9:1;
the composite complexing agent takes a porous material as a carrier, and the loading mass ratio is 3-7:2-6:1, sodium ethylenediamine tetramethylene phosphate, sodium diethylenetriamine pentamethylene phosphonate and polyhydroxyacrylic acid;
the preparation method of the stripping solution comprises the steps of sequentially dissolving an oxidant, a composite complexing agent, a corrosion inhibitor, a penetrating agent and an auxiliary agent in water, stirring for 5-15min, adding water to a constant volume of 1L, continuously adding a buffering agent, controlling the PH to be 3.5-5, continuously stirring for 10-20min, and slowly heating to 20-35 ℃ during the period.
2. The stripping solution for PCB manufacturing process as set forth in claim 1, wherein: the preparation method of the composite complexing agent specifically comprises the following steps:
(1) Weighing 10-20 parts of mixture of ethylenediamine tetra (sodium methylene phosphate), diethylenetriamine penta (sodium methylene phosphonate) and polyhydroxyacrylic acid according to the mass ratio, ball milling for 20-30min, adding into 50-100 times of water, and uniformly stirring;
(2) Adding 10 times of porous material in the mixture, ultrasonic dispersing at 15-25KHz frequency for 1-2h, and standing for adsorption for 24h;
(3) Centrifuging at 50-100rpm for 20-30min, standing for 5min, switching to 500-1000rpm for 10-15min, standing for 20min, switching to 2000-3000rpm for 3-5min, centrifuging, removing supernatant, and oven drying precipitate at 30-50deg.C; the porous material is one or a mixture of multiple kinds of biochar, molecular sieve and diatomite.
3. The stripping solution for PCB manufacturing process as set forth in claim 1, wherein: the preparation method of the corrosion inhibitor comprises the following raw materials, by weight, 3-9 parts of a colored benzothiazole, 3-7 parts of a benzotriazole, 5-15 parts of a methylbenzotriazole, 1-3 parts of an activation modifier and 20-30 parts of an ethanol solution, wherein the raw materials comprise the following specific components:
(1) Mixing the azyl benzothiazole, the benzotriazole and the methylbenzotriazole, and grinding and refining for 15-25min to obtain a grinding mixture;
(2) Adding the grinding mixture into ethanol solution, stirring and dispersing at 200-400rpm for 30min, and dispersing the solution;
(3) Adding an activating modifier into the dispersion liquid while stirring, slowly heating to 50 ℃, and continuously stirring for 20-40min to obtain the modified polyurethane foam.
4. A stripping solution for a PCB process as claimed in claim 3, wherein: the mass ratio of the activation modifier is 2-6: 1-butyl-2-methylimidazole, a mixture of biological enzymes; the biological enzyme is a mixture of lignin enzyme, pectase and lysozyme in a mass ratio of 1:1:1; the mass fraction of the ethanol solution is 30-60%.
5. An penetrant for use in the stripping solution as claimed in any of claims 1 to 4, characterized in that: the preparation method of the penetrating agent comprises the following raw materials, by weight, 15-20 parts of sodium alkylbenzenesulfonate, 5-8 parts of sulfonated oil and 15-30 parts of strengthening modifier, wherein the raw materials comprise the following concrete steps:
(1) Mixing sodium alkylbenzenesulfonate with sulfonated oil, and uniformly stirring;
(2) Adding reinforcing modifier, stirring and dispersing for 30min, stopping stirring, and introducing N 2 Controlling the air flow to be 200-400mL/min, performing ultrasonic dispersion at 20-30KHz, and stopping ventilation after 2 h.
6. The penetrant of claim 5, wherein: the strengthening modifier is a mixture of linoleoyl diethanolamine and soyate diethanolamine with the mass ratio of 1:1-3.
7. A method of using the stripping solution as claimed in claim 5, characterized in that: the specific steps are as follows,
(1) Soaking the deplating piece in water at 40-60deg.C for 3-5min;
(2) Taking out, transferring to a deplating solution with the temperature of 20-35 ℃, electrifying and electrolyzing at the voltage of 6-12V for 1-4min;
(3) Taking out, ultrasonic cleaning with water, and oven drying at 30-40deg.C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310176800.8A CN116145226A (en) | 2023-02-28 | 2023-02-28 | Stripping solution for PCB (printed circuit board) manufacturing process and application method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310176800.8A CN116145226A (en) | 2023-02-28 | 2023-02-28 | Stripping solution for PCB (printed circuit board) manufacturing process and application method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116145226A true CN116145226A (en) | 2023-05-23 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310176800.8A Pending CN116145226A (en) | 2023-02-28 | 2023-02-28 | Stripping solution for PCB (printed circuit board) manufacturing process and application method thereof |
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| Country | Link |
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| CN (1) | CN116145226A (en) |
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2023
- 2023-02-28 CN CN202310176800.8A patent/CN116145226A/en active Pending
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