CN114449769B - Single-sided PCB (printed circuit board) and processing technology thereof - Google Patents
Single-sided PCB (printed circuit board) and processing technology thereof Download PDFInfo
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- CN114449769B CN114449769B CN202210147141.0A CN202210147141A CN114449769B CN 114449769 B CN114449769 B CN 114449769B CN 202210147141 A CN202210147141 A CN 202210147141A CN 114449769 B CN114449769 B CN 114449769B
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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
- H05K3/0091—Apparatus for coating printed circuits using liquid non-metallic coating compositions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/12—Stencil printing; Silk-screen printing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M7/00—After-treatment of prints, e.g. heating, irradiating, setting of the ink, protection of the printed stock
- B41M7/0081—After-treatment of prints, e.g. heating, irradiating, setting of the ink, protection of the printed stock using electromagnetic radiation or waves, e.g. ultraviolet radiation, electron beams
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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
- H05K3/0011—Working of insulating substrates or insulating layers
- H05K3/0044—Mechanical working of the substrate, e.g. drilling or punching
- H05K3/0047—Drilling of holes
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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
- H05K3/0011—Working of insulating substrates or insulating layers
- H05K3/0044—Mechanical working of the substrate, e.g. drilling or punching
- H05K3/005—Punching of holes
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Abstract
The invention discloses a single-sided PCB (printed circuit board) and a processing technology thereof, which comprises the following processes: (1) pretreatment: cutting and cleaning the copper-clad substrate; (2) preparing a circuit: printing a circuit pattern, carrying out UV drying, etching and film stripping; (3) solder resist printing: coating solder resist ink and carrying out UV drying; (3) printing of characters: printing characters on the back and the front of the copper-clad substrate, and performing UV drying; (5) and (3) post-treatment: and (6) drilling a positioning hole and punching. The dicyclopentadiene and benzothiazole are introduced into the molecular structure of the cured resin, so that the low-molecular-polarization-rate and low-dielectric-constant resin has low molar polarization rate; when the epoxy resin is cured in a synergistic manner, the crosslinking density is reduced due to the large steric hindrance effect of the epoxy resin, a cured product with larger molecular space gap and lower density is formed, and the improvement of the dielectric property of the cured resin and the cured epoxy resin is facilitated; meanwhile, the strong electron-withdrawing ability of the solder mask can enhance the bonding performance between the solder mask and the circuit pattern.
Description
Technical Field
The invention relates to the technical field of circuit boards, in particular to a single-sided PCB (printed circuit board) and a processing technology thereof.
Background
The PCB, also called a printed circuit board, is an important electronic component of electronic components and is a carrier for electrical interconnection of the electronic components; after a circuit pattern is formed by printing, solder resist ink is coated on a non-welding part on the surface of the circuit board in a screen printing mode, a gravure printing mode or an ink-jet printing mode, and then a solder resist ink protection layer is formed by curing to protect the circuit. With the advent of the 5G era, electronic information products have evolved into the gigahertz (GHz) era, and high-speed printed circuits have become a focus of research. It has been found that some solder resist inks cause signal transmission loss in printed wiring boards. Therefore, we propose a single-sided PCB printed circuit board and its processing technology.
Disclosure of Invention
The invention aims to provide a single-sided PCB and a processing technology thereof, which aim to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: a processing technology of a single-sided PCB printed circuit board comprises the following processes:
(1) pretreatment: cutting and cleaning the copper-clad substrate;
(2) preparing a circuit: printing a circuit pattern, carrying out UV drying, etching and film stripping;
(3) Solder resist printing: coating solder resist ink and carrying out UV drying;
(3) printing of characters: printing characters on the back and the front of the copper-clad substrate, and performing UV drying;
(5) and (3) post-treatment: and (6) drilling a positioning hole and punching.
Further, the solder resist ink comprises the following components in parts by weight: the component A comprises: 40-60 parts of curing resin, 25-45 parts of titanium dioxide, 0-15 parts of barium sulfate, 4-7 parts of photoinitiator and 2-7 parts of auxiliary agent;
and B component: 25-40 parts of epoxy resin, 0-20 parts of titanium dioxide, 2-5 parts of fumed silica, 20-45 parts of diluent, 5-12 parts of auxiliary agent and 15-30 parts of solvent.
Further, the cured resin is prepared by the following process:
1.1. mixing dicyclopentadiene and aluminum chloride, heating to 120-130 ℃ in a nitrogen atmosphere, and preserving heat for 1.6-2.5 h; slowly adding divinylbenzene, and reacting for 3.6-4.5 hours under heat preservation; adding a 5% sodium hydroxide solution, stirring for 50-75 min, filtering and washing; distilling the organic phase; dissolving toluene, extracting with deionized water, repeating for many times, and distilling to obtain dicyclopentadiene derivative A; divinylbenzene and dicyclopentadiene are added, reactive double bonds are introduced into a dicyclopentadiene structure, and the dicyclopentadiene with an alicyclic structure is introduced into the prepared cured resin, so that the thermal stability of the resin is improved, the crosslinking density is increased, and the free motion and polarization of a molecular chain can be limited; and the dicyclopentadiene is a large steric hindrance group, so that the number of polarized molecules in unit volume is reduced, and the dicyclopentadiene has higher free volume, thereby reducing the dielectric constant of the prepared cured resin.
1.2. Taking 2, 2-bis [ (3-amido-4-hydroxyl) phenyl]Hexafluoropropane, Et3N, Sm (OTf) 3 Mixing, adding an ethanol water solution, slowly adding 4-vinylbenzaldehyde at the temperature of 75-85 ℃ in a nitrogen atmosphere, and carrying out reflux reaction for 10-15 h; adding deionized water after reaction, and performing suction filtration to obtain a benzothiazole derivative B; aldehyde group reacts with amino and phenolic hydroxyl to obtain benzothiazole functional group with lower low dielectric constant and low dielectric lossA factor; the movement and orientation of the chain segments are limited by curing the crosslinking network, and the prepared cured resin can show more excellent low dielectric property after crosslinking and curing.
1.3. Heating acetone to 80-100 ℃ in a nitrogen atmosphere; slowly dropwise adding a mixed monomer of the dicyclopentadiene derivative A, the benzothiazole derivative B, the initiator and the chain transfer agent, and finishing dropwise adding for 2-3 h; reacting for 2-4 h at the temperature of 85-100 ℃ in a heat preservation manner; heating to 95-115 ℃, and reacting for 1-2 h; and heating to 115-125 ℃, and continuing to react for 60-90 min for 1-2 h to obtain the cured resin. And carrying out double bond addition polymerization on the dicyclopentadiene derivative A and the benzothiazole derivative B to obtain a polymer containing dicyclopentadiene and benzothiazole bifunctional groups, and curing the epoxy resin by unreacted amino in the benzothiazole derivative B to obtain the cured resin.
In the technical scheme, fluorine is introduced into the molecular structure of the cured resin, and has strong electronegativity, so that electrons can be firmly bound to form a C-F bond, namely a low-polarity atomic group, so as to reduce the molecular polarizability; meanwhile, dicyclopentadiene and benzothiazole are introduced, and difunctional groups with low molar polarizability are used as large steric hindrance groups, so that the number of polarized molecules in unit volume can be reduced, the free volume is higher, the material density is reduced, and the dielectric constant of the prepared cured resin is reduced. Meanwhile, the thermal stability of the prepared cured resin is enhanced; the dicyclopentadiene derivative A contains a bi-alicyclic chain segment, so that the water resistance of the cured resin is further improved due to the hydrophobicity; when the epoxy resin is cured, due to the large steric hindrance effect of the dicyclopentadiene and the benzothiazole, the crosslinking density is reduced, and the improvement of the dielectric property of the cured resin and the cured epoxy resin is facilitated;
furthermore, the molar ratio of the divinylbenzene, the aluminum chloride, the dicyclopentadiene and the sodium hydroxide solution is 1 (0.020-0.022), 0.013-0.015 and 0.083-0.085.
Further, the molar ratio of the 2, 2-bis [ (3-amino-4-hydroxy) phenyl ] hexafluoropropane to the 4-vinylbenzaldehyde to Et3N to Sm (OTf)3 is 1 (1.2-1.5) to (1.6-2.0) to (0.16-0.20).
Furthermore, the mass ratio of the acetone, the dicyclopentadiene derivative A, the benzothiazole derivative B, the initiator and the chain transfer agent is (41-67): (20-45): (15-35): (0.5-3.0): (0.1-0.5).
Further, the epoxy resin is prepared by the following process:
2.1. mixing 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone and toluene, adding trifluoromethanesulfonic acid, stirring, and reacting for 72 h; pouring into ice water, separating an organic phase, washing by using 5% sodium bicarbonate water solution and distilled water, distilling, and recrystallizing and purifying by using petroleum ether to obtain a dimethyl product A;
mixing the product A, pyridine and distilled water, heating and refluxing, and reacting for 3-4 h; adding potassium permanganate, and stirring and reacting for 2.7-3.2 h; filtering, concentrating, adding a sodium hydroxide aqueous solution, and heating and refluxing for 2-4 h; adding potassium permanganate again, and refluxing for 2.7-3.2 h; cooling to 60-72 ℃, slowly adding ethanol, and refluxing for 50-70 min; filtering, concentrating, adjusting the pH to 1-2 by using dilute hydrochloric acid, filtering, washing by using dilute hydrochloric acid salt and distilled water, and drying in vacuum to obtain a diacid product B;
mixing the diacid product B, thionyl chloride and N, N-dimethylformamide, stirring and refluxing for 5.6-6.4 h, carrying out vacuum distillation, cooling, filtering, and recrystallizing and purifying anhydrous petroleum ether to obtain a diacyl chloride product C;
2.2. Taking toluene, adding a diacyl chloride product C, 1,3, 5-tri (2-hydroxyethyl) -1,3, 5-triazine-2, 4, 6-trione and p-toluenesulfonic acid, heating to reflux under the protection of nitrogen, and reacting for 3-4 h; cooling to room temperature, washing with 5% sodium bicarbonate water solution and distilled water, drying the organic layer, filtering, and rotary evaporating to obtain ester D;
2.3. dissolving glycidol in benzene, adding triethylamine, adjusting the temperature of the system to 0 ℃, slowly adding the esterified substance D, stirring for 4-5 h, and standing for 20-24 h at room temperature; filtering, concentrating, washing with 5% sodium bicarbonate ice water solution and distilled water, and drying to obtain the epoxy resin.
In the technical scheme, 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone and toluene react under the action of trifluoromethane sulfonic acid to obtain a product A with three benzene rings, two methyl groups and one trifluoromethyl group; oxidizing methyl in the product A to generate carboxyl, and then performing acyl chlorination to obtain a product C with two acyl chloride groups; reacting the modified epoxy resin with 1,3, 5-tri (2-hydroxyethyl) -1,3, 5-triazine-2, 4, 6-trione, and grafting acyl chloride and hydroxyl to obtain an ester (ester D) with a branched structure, so as to improve the toughness, bending strength and impact strength of the epoxy resin; the residual acyl chloride group reacts with hydroxyl in glycidol to obtain the epoxy terminated branched epoxy resin with high thermal stability, dielectric property and water resistance.
Further, the molar ratio of the 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone to the toluene to the trifluoromethanesulfonic acid is 1:8: 0.8;
furthermore, the molar ratio of the product A, the pyridine to the potassium permanganate to be added again to the sodium hydroxide is 1 (51-52) to 6:5 (14.0-14.4).
Furthermore, the molar ratio of the diacid product B to the thionyl chloride is 1 (45-47).
Furthermore, the molar ratio of the diacyl chloride product C, 1,3, 5-tri (2-hydroxyethyl) -1,3, 5-triazine-2, 4, 6-trione and p-toluenesulfonic acid is (3.05-3.10) to 1 (0.023-0.046).
Furthermore, the molar ratio of the glycidol, the triethylamine and the ester D is (2.2-2.4): 2.1-2.3): 1.
Further, the auxiliary agent is lubricant OP wax.
Further, the preparation process of the solder resist ink comprises the following steps:
respectively dispersing the component A and the component B at high speed for 30-80 min under the conditions of sealing and keeping out of the sun, and controlling the temperature to be below 65 ℃; grinding to below 5 μm.
Further, the solder resist printing process comprises the following steps:
taking solder resist ink for screen printing; baking at 80 deg.C for 30 min; carrying out UV curing; developing in a developing solution with the concentration of sodium carbonate of 0.8-1.2%; baking at 160 ℃ for 1 h; and obtaining the solder mask.
Compared with the prior art, the invention has the following beneficial effects:
according to the single-sided PCB and the processing technology thereof, fluorine is introduced into the molecular structure of the cured resin, and has strong electronegativity, so that electrons can be firmly bound to form a C-F bond, namely a low-polarity atomic group, so that the molecular polarizability is reduced; meanwhile, dicyclopentadiene and benzothiazole are introduced, and difunctional groups with low molar polarizability are used as large steric hindrance groups, so that the number of polarized molecules in unit volume can be reduced, the free volume is higher, the material density is reduced, and the dielectric constant of the prepared cured resin is reduced; when the modified dicyclopentadiene and the epoxy resin are cured in a synergistic manner, due to the large steric hindrance effect of the dicyclopentadiene and the benzothiazole, the crosslinking density is reduced, a cured product with larger molecular space gap and lower density is formed, and the modified dicyclopentadiene and epoxy resin cured dielectric property is improved; meanwhile, the bonding property of the manufactured solder mask can be enhanced due to the strong electron-withdrawing capability.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A processing technology of a single-sided PCB printed circuit board comprises the following processes:
(1) pretreatment: cutting the copper-clad substrate into small materials; cleaning, cleaning and roughening the surface copper foil, and keeping the surface clean;
(2) preparing a circuit: taking circuit ink, and transferring a circuit pattern onto a copper-clad substrate through screen printing; curing by ultraviolet rays; etching to remove the redundant copper foil; removing the film; cleaning, roughening and drying the surface copper foil;
(3) solder resist printing:
respectively dispersing the component A and the component B at high speed for 60min under sealed and dark conditions, and controlling the temperature below 65 ℃; grinding to below 5 μm;
taking solder resist ink for screen printing; baking at 80 deg.C for 30 min; carrying out UV curing; developing in a developing solution with the concentration of sodium carbonate of 1 percent; baking for 1h at 160 ℃ to obtain a solder mask; the thickness of the solder resist ink is 20 μm;
(3) printing of characters: printing characters on the back and the front of the copper-clad substrate, and curing by ultraviolet rays; air cooling;
(5) and (3) post-treatment: drilling a positioning hole, preheating, punching a plate, pressing the hole and V-cutting.
Example 1
The solder resist ink comprises the following components in parts by weight: the component A comprises: 40 parts of curing resin, 25 parts of titanium dioxide, 4 parts of photoinitiator and 2 parts of auxiliary agent; and B component: 25 parts of epoxy resin, 2 parts of fumed silica, 20 parts of diluent, 5 parts of auxiliary agent and 15 parts of solvent;
The cured resin is prepared by the following process:
1.1. mixing dicyclopentadiene and aluminum chloride, heating to 120 ℃ in a nitrogen atmosphere, and keeping the temperature for 1.6 h; slowly adding divinylbenzene, and reacting for 3.6 hours under heat preservation; adding 5% sodium hydroxide solution, stirring for 50min, filtering, and washing; distilling the organic phase; dissolving toluene, extracting with deionized water, repeating for many times, and distilling to obtain dicyclopentadiene derivative A;
1.2. mixing 2, 2-bis [ (3-amino-4-hydroxy) phenyl ] hexafluoropropane, Et3N and Sm (OTf)3, adding an ethanol aqueous solution, slowly adding 4-vinylbenzaldehyde at 75 ℃ in a nitrogen atmosphere, and carrying out reflux reaction for 10 hours; adding deionized water after reaction, and performing suction filtration to obtain a benzothiazole derivative B;
1.3. heating acetone to 80 ℃ in a nitrogen atmosphere; slowly dripping mixed monomers of the dicyclopentadiene derivative A, the benzothiazole derivative B, the initiator and the chain transfer agent, and finishing dripping within 2 hours; keeping the temperature at 85 ℃ and reacting for 2 h; heating to 95 ℃ and reacting for 1 h; heating to 115 ℃, and continuing to react for 60min for 1h to obtain cured resin;
the molar ratio of the divinylbenzene to the aluminum chloride to the dicyclopentadiene to the sodium hydroxide solution is 1:0.020:0.013: 0.083; the molar ratio of 2, 2-bis [ (3-amino-4-hydroxy) phenyl ] hexafluoropropane, 4-vinylbenzaldehyde, Et3N, Sm (OTf)3 is 1:1.2:1.6: 0.16; the mass ratio of acetone to the dicyclopentadiene derivative A to the benzothiazole derivative B to the initiator to the chain transfer agent is 41:20:15:0.5: 0.1;
The epoxy resin is prepared by the following process:
2.1. mixing 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone and toluene, adding trifluoromethanesulfonic acid, stirring, and reacting for 72 h; pouring into ice water, separating an organic phase, washing by using 5% sodium bicarbonate water solution and distilled water, distilling, and recrystallizing and purifying by using petroleum ether to obtain a dimethyl product A;
mixing the product A, pyridine and distilled water, heating and refluxing, and reacting for 3 hours; adding potassium permanganate, and stirring to react for 2.7 h; filtering, concentrating, adding sodium hydroxide water solution, heating and refluxing for 2 h; adding potassium permanganate again, and refluxing for 2.7 h; cooling to 60 deg.C, slowly adding ethanol, and refluxing for 50 min; filtering, concentrating, adjusting the pH to 2 by using dilute hydrochloric acid, filtering, washing by using dilute hydrochloric acid and distilled water, and drying in vacuum to obtain a diacid product B;
mixing the diacid product B, thionyl chloride and N, N-dimethylformamide, stirring and refluxing for 5.6 hours, carrying out vacuum distillation, cooling, filtering, and recrystallizing and purifying anhydrous petroleum ether to obtain a diacyl chloride product C;
2.2. taking toluene, adding a diacid chloride product C, 1,3, 5-tri (2-hydroxyethyl) -1,3, 5-triazine-2, 4, 6-trione and p-toluenesulfonic acid, heating to reflux under the protection of nitrogen, and reacting for 3 hours; cooling to room temperature, washing with 5% sodium bicarbonate water solution and distilled water, drying the organic layer, filtering, and rotary evaporating to obtain ester D;
2.3. Dissolving glycidol in benzene, adding triethylamine, adjusting the temperature of the system to 0 ℃, slowly adding the esterified substance D, stirring for 4 hours, and standing for 20 hours at room temperature; filtering, concentrating, washing with 5% sodium bicarbonate ice water solution and distilled water, and drying to obtain epoxy resin;
the mol ratio of the 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone to the toluene to the trifluoromethane sulfonic acid is 1:8: 0.8; the molar ratio of the product A, pyridine, potassium permanganate and potassium permanganate added again to sodium hydroxide is 1:51:6:5: 14.0; the molar ratio of the diacid product B to the thionyl chloride is 1: 45; the molar ratio of the diacid chloride product C, the 1,3, 5-tri (2-hydroxyethyl) -1,3, 5-triazine-2, 4, 6-trione and the p-toluenesulfonic acid is 3.05:1: 0.023; the molar ratio of the glycidol to the triethylamine to the ester D is 2.2:2.1: 1;
example 2
The solder resist ink comprises the following components in parts by weight: the component A comprises: 50 parts of curing resin, 35 parts of titanium dioxide, 7 parts of barium sulfate, 5 parts of photoinitiator and 4 parts of auxiliary agent; and B component: 32 parts of epoxy resin, 10 parts of titanium dioxide, 3 parts of fumed silica, 32 parts of diluent, 8 parts of auxiliary agent and 22 parts of solvent;
the cured resin is prepared by the following process:
1.1. mixing dicyclopentadiene and aluminum chloride, heating to 125 ℃ in a nitrogen atmosphere, and keeping the temperature for 2 hours; slowly adding divinylbenzene, and reacting for 4 hours under heat preservation; adding 5% sodium hydroxide solution, stirring for 64min, filtering, and washing; distilling the organic phase; dissolving toluene, extracting with deionized water, repeating for many times, and distilling to obtain dicyclopentadiene derivative A;
1.2. Mixing 2, 2-bis [ (3-amino-4-hydroxy) phenyl ] hexafluoropropane, Et3N and Sm (OTf)3, adding an ethanol aqueous solution, slowly adding 4-vinylbenzaldehyde at the temperature of 80 ℃ in a nitrogen atmosphere, and carrying out reflux reaction for 12 hours; adding deionized water after reaction, and performing suction filtration to obtain a benzothiazole derivative B;
1.3. heating acetone to 90 ℃ in a nitrogen atmosphere; slowly dripping mixed monomers of the dicyclopentadiene derivative A, the benzothiazole derivative B, the initiator and the chain transfer agent, and finishing dripping within 2.5 hours; keeping the temperature at 92 ℃ and reacting for 3 hours; heating to 105 ℃, and reacting for 1.5 h; heating to 120 ℃, and continuing to react for 75min to obtain cured resin;
the molar ratio of divinylbenzene to aluminum chloride to dicyclopentadiene to sodium hydroxide solution is 1:0.021:0.014: 0.084; the molar ratio of 2, 2-bis [ (3-amino-4-hydroxy) phenyl ] hexafluoropropane, 4-vinylbenzaldehyde, Et3N, Sm (OTf)3 is 1:1.3:1.8: 0.18; the mass ratio of acetone, the dicyclopentadiene derivative A, the benzothiazole derivative B, the initiator and the chain transfer agent is 54:32:25:1.5: 0.3;
the epoxy resin is prepared by the following process:
2.1. mixing 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone and toluene, adding trifluoromethanesulfonic acid, stirring, and reacting for 72 h; pouring into ice water, separating an organic phase, washing by using 5% sodium bicarbonate water solution and distilled water, distilling, and recrystallizing and purifying by using petroleum ether to obtain a dimethyl product A;
Mixing the product A, pyridine and distilled water, heating and refluxing, and reacting for 3.5 hours; adding potassium permanganate, and stirring for reaction for 3 hours; filtering, concentrating, adding sodium hydroxide water solution, heating and refluxing for 3 h; adding potassium permanganate again, and refluxing for 3 h; cooling to 66 deg.C, slowly adding ethanol, and refluxing for 60 min; filtering, concentrating, adjusting pH to 1.5 with dilute hydrochloric acid, filtering, washing with dilute hydrochloride and distilled water, and vacuum drying to obtain diacid product B;
mixing the diacid product B, thionyl chloride and N, N-dimethylformamide, stirring and refluxing for 6 hours, carrying out vacuum distillation, cooling, filtering, and recrystallizing and purifying anhydrous petroleum ether to obtain a diacyl chloride product C;
2.2. taking toluene, adding a diacid chloride product C, 1,3, 5-tri (2-hydroxyethyl) -1,3, 5-triazine-2, 4, 6-trione and p-toluenesulfonic acid, heating to reflux under the protection of nitrogen, and reacting for 3.5 hours; cooling to room temperature, washing with 5% sodium bicarbonate water solution and distilled water, drying the organic layer, filtering, and rotary evaporating to obtain ester D;
2.3. dissolving glycidol in benzene, adding triethylamine, adjusting the temperature of the system to 0 ℃, slowly adding the esterified substance D, stirring for 4.5h, and standing for 22h at room temperature; filtering, concentrating, washing with 5% sodium bicarbonate ice water solution and distilled water, and drying to obtain epoxy resin;
The molar ratio of the 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone to the toluene to the trifluoromethanesulfonic acid is 1:8: 0.8; the molar ratio of the product A, pyridine, potassium permanganate and potassium permanganate added again to sodium hydroxide is 1:52:6:5: 14.2; the molar ratio of the diacid product B to the thionyl chloride is 1: 46; the molar ratio of the diacid chloride product C, 1,3, 5-tri (2-hydroxyethyl) -1,3, 5-triazine-2, 4, 6-trione and p-toluenesulfonic acid is 3.07:1: 0.033; the molar ratio of glycidol, triethylamine and ester D is 2.3:2.2: 1.
Example 3
The solder resist ink comprises the following components in parts by weight: the component A comprises: 60 parts of curing resin, 45 parts of titanium dioxide, 15 parts of barium sulfate, 7 parts of photoinitiator and 7 parts of auxiliary agent; and B component: 40 parts of epoxy resin, 20 parts of titanium dioxide, 5 parts of fumed silica, 45 parts of diluent, 12 parts of auxiliary agent and 30 parts of solvent;
the cured resin is prepared by the following process:
1.1. mixing dicyclopentadiene and aluminum chloride, heating to 130 ℃ in a nitrogen atmosphere, and keeping the temperature for 2.5 hours; slowly adding divinylbenzene, and reacting for 4.5 hours under heat preservation; adding 5% sodium hydroxide solution, stirring for 75min, filtering, and washing; distilling the organic phase; dissolving toluene, extracting with deionized water, repeating for many times, and distilling to obtain dicyclopentadiene derivative A;
1.2. Mixing 2, 2-bis [ (3-amino-4-hydroxy) phenyl ] hexafluoropropane, Et3N and Sm (OTf)3, adding an ethanol aqueous solution, slowly adding 4-vinylbenzaldehyde at the temperature of 85 ℃ in a nitrogen atmosphere, and carrying out reflux reaction for 15 hours; adding deionized water after reaction, and performing suction filtration to obtain a benzothiazole derivative B;
1.3. heating acetone to 100 ℃ in a nitrogen atmosphere; slowly dripping mixed monomers of the dicyclopentadiene derivative A, the benzothiazole derivative B, the initiator and the chain transfer agent, and finishing dripping within 3 hours; keeping the temperature at 100 ℃ and reacting for 4 hours; heating to 115 ℃ and reacting for 2 h; heating to 125 ℃, and continuing to react for 90min for 2h to obtain cured resin;
the molar ratio of divinylbenzene to aluminum chloride to dicyclopentadiene to sodium hydroxide solution is 1:0.022:0.015: 0.085; the molar ratio of 2, 2-bis [ (3-amino-4-hydroxy) phenyl ] hexafluoropropane, 4-vinylbenzaldehyde, Et3N, Sm (OTf)3 is 1:1.5:2.0: 0.20; the mass ratio of acetone to the dicyclopentadiene derivative A to the benzothiazole derivative B to the initiator to the chain transfer agent is 67:45:35:3.0: 0.5;
the epoxy resin is prepared by the following process:
2.1. mixing 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone and toluene, adding trifluoromethanesulfonic acid, stirring, and reacting for 72 h; pouring into ice water, separating an organic phase, washing by using 5% sodium bicarbonate water solution and distilled water, distilling, and recrystallizing and purifying by using petroleum ether to obtain a dimethyl product A;
Mixing the product A, pyridine and distilled water, heating and refluxing, and reacting for 4 hours; adding potassium permanganate, and stirring to react for 3.2 h; filtering, concentrating, adding sodium hydroxide water solution, heating and refluxing for 4 h; adding potassium permanganate again, and refluxing for 3.2 h; cooling to 72 deg.C, slowly adding ethanol, and refluxing for 70 min; filtering, concentrating, adjusting pH to 1 with dilute hydrochloric acid, filtering, washing with dilute hydrochloric acid and distilled water, and vacuum drying to obtain diacid product B;
mixing the diacid product B, thionyl chloride and N, N-dimethylformamide, stirring and refluxing for 6.4h, carrying out vacuum distillation, cooling, filtering, and recrystallizing and purifying anhydrous petroleum ether to obtain a diacyl chloride product C;
2.2. taking toluene, adding a diacid chloride product C, 1,3, 5-tri (2-hydroxyethyl) -1,3, 5-triazine-2, 4, 6-trione and p-toluenesulfonic acid, heating to reflux under the protection of nitrogen, and reacting for 4 hours; cooling to room temperature, washing with 5% sodium bicarbonate water solution and distilled water, drying the organic layer, filtering, and rotary evaporating to obtain ester D;
2.3. dissolving glycidol in benzene, adding triethylamine, adjusting the temperature of the system to 0 ℃, slowly adding the esterified substance D, stirring for 5 hours, and standing for 24 hours at room temperature; filtering, concentrating, washing with 5% sodium bicarbonate ice water solution and distilled water, and drying to obtain epoxy resin;
The molar ratio of the 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone to the toluene to the trifluoromethanesulfonic acid is 1:8: 0.8; the molar ratio of the product A, pyridine, potassium permanganate and potassium permanganate added again to sodium hydroxide is 1:52:6:5: 14.4; the molar ratio of the diacid product B to the thionyl chloride is 1: 47; the mole ratio of the diacid chloride product C, 1,3, 5-tri (2-hydroxyethyl) -1,3, 5-triazine-2, 4, 6-trione and p-toluenesulfonic acid is 3.10:1: 0.046; the molar ratio of glycidol, triethylamine and ester D is 2.4:2.3: 1.
Comparative example 1
The cured resin is prepared by the following process:
1.1. mixing dicyclopentadiene and aluminum chloride, heating to 120 ℃ in a nitrogen atmosphere, and keeping the temperature for 1.6 h; slowly adding divinylbenzene, and reacting for 3.6 hours under heat preservation; adding 5% sodium hydroxide solution, stirring for 50min, filtering, and washing; distilling the organic phase; dissolving toluene, extracting with deionized water, repeating for many times, and distilling to obtain dicyclopentadiene derivative A;
1.2. heating acetone to 80 ℃ in a nitrogen atmosphere; slowly dripping mixed monomers of the dicyclopentadiene derivative A, the aminostyrene, the initiator and the chain transfer agent for 2 hours; keeping the temperature at 85 ℃ and reacting for 2 h; heating to 95 ℃ and reacting for 1 h; heating to 115 ℃, and continuing to react for 60min for 1h to obtain cured resin;
The molar ratio of divinylbenzene to aluminum chloride to dicyclopentadiene to sodium hydroxide solution is 1:0.020:0.013: 0.083; the mass ratio of acetone to the dicyclopentadiene derivative A to the aminostyrene to the initiator to the chain transfer agent is 41:20:15:0.5: 0.1;
other processes and steps are the same as those of example 1.
Comparative example 2
The cured resin is prepared by the following process:
1.1. mixing 2, 2-bis [ (3-amino-4-hydroxy) phenyl ] hexafluoropropane, Et3N and Sm (OTf)3, adding an ethanol aqueous solution, slowly adding 4-vinylbenzaldehyde at 75 ℃ in a nitrogen atmosphere, and carrying out reflux reaction for 10 hours; adding deionized water after reaction, and performing suction filtration to obtain a benzothiazole derivative B;
1.2. heating acetone to 80 ℃ in a nitrogen atmosphere; slowly dropwise adding a mixed monomer of the aminostyrene, the benzothiazole derivative B, the initiator and the chain transfer agent, and finishing dropwise adding within 2 h; keeping the temperature at 85 ℃ and reacting for 2 h; heating to 95 ℃ and reacting for 1 h; heating to 115 ℃, and continuing to react for 60min for 1h to obtain cured resin;
the molar ratio of 2, 2-bis [ (3-amino-4-hydroxy) phenyl ] hexafluoropropane, 4-vinylbenzaldehyde, Et3N, Sm (OTf)3 is 1:1.2:1.6: 0.16; the mass ratio of acetone, aminostyrene, benzothiazole derivative B, initiator and chain transfer agent is 41:20:15:0.5: 0.1;
Other processes and steps are the same as those of example 1.
Comparative example 3
Taking a polystyrene-polydopamine composite material as a curing resin;
other processes and steps are the same as those of example 1.
Comparative example 4
The epoxy resin is prepared by the following process:
2.1. mixing 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone and toluene, adding trifluoromethanesulfonic acid, stirring, and reacting for 72 h; pouring into ice water, separating an organic phase, washing by using 5% sodium bicarbonate water solution and distilled water, distilling, and recrystallizing and purifying by using petroleum ether to obtain a dimethyl product A;
mixing the product A, pyridine and distilled water, heating and refluxing, and reacting for 3 hours; adding potassium permanganate, and stirring to react for 2.7 h; filtering, concentrating, adding sodium hydroxide water solution, heating and refluxing for 2 h; adding potassium permanganate again, and refluxing for 2.7 h; cooling to 60 deg.C, slowly adding ethanol, and refluxing for 50 min; filtering, concentrating, adjusting pH to 2 with dilute hydrochloric acid, filtering, washing with dilute hydrochloric acid and distilled water, and vacuum drying to obtain diacid product B;
mixing the diacid product B, thionyl chloride and N, N-dimethylformamide, stirring and refluxing for 5.6 hours, carrying out vacuum distillation, cooling, filtering, and recrystallizing and purifying anhydrous petroleum ether to obtain a diacyl chloride product C;
2.2. Dissolving glycidol in benzene, adding triethylamine, adjusting the temperature of the system to 0 ℃, slowly adding the diacyl chloride product C, stirring for 4 hours, and standing for 20 hours at room temperature; filtering, concentrating, washing with 5% sodium bicarbonate ice water solution and distilled water, and drying to obtain epoxy resin;
the mol ratio of the 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone to the toluene to the trifluoromethane sulfonic acid is 1:8: 0.8; the molar ratio of the product A, pyridine, potassium permanganate and potassium permanganate added again to sodium hydroxide is 1:51:6:5: 14.0; the molar ratio of the diacid product B to the thionyl chloride is 1: 45; the molar ratio of the glycidol, the triethylamine and the diacyl chloride product C is 2.2:2.1: 1;
other processes and steps are the same as those of comparative example 3.
Comparative example 5
Taking a polystyrene-polydopamine composite material as a curing resin; bisphenol a type epoxy resin as an epoxy resin;
other processes and steps are the same as those of example 1.
Experiment of
Samples were prepared from the solder resist layers and the printed wiring boards obtained in examples 1 to 3 and comparative examples 1 to 5, and the properties thereof were measured and the measurement results were recorded:
dielectric properties: according to GB/T1409-2006, the dielectric property of the sample under 1MHz is tested;
peel strength: the peel strength of the test specimens was determined in accordance with GB/T4722-2017.
| Dielectric constant (1MHz) | Loss factor (1MHz) | Peel strength (N/mm) | |
| Example 1 | 3.05 | 0.0080 | 5.3 |
| Example 2 | 2.84 | 0.0072 | 5.4 |
| Example 3 | 2.67 | 0.0066 | 5.8 |
| Comparative example 1 | 3.18 | 0.0100 | 4.4 |
| Comparative example 2 | 3.21 | 0.0120 | 4.7 |
| Comparative example 3 | 3.56 | 0.026 | 3.8 |
| Comparative example 4 | 3.84 | 0.034 | 3.2 |
| Comparative example 5 | 4.05 | 0.037 | 2.7 |
From the data in the table above, it is clear that the following conclusions can be drawn:
as a result of comparing the solder resist layers obtained in examples 1 to 3 with those obtained in comparative examples 1 to 5, it was found that,
1. compared with the comparative example 5, the dielectric constant and the loss factor data of the solder mask obtained in the examples 1 to 3 are lower, which fully shows that the application realizes the improvement of the dielectric property and the bonding property of the solder mask;
2. the solder resist obtained in comparative examples 1 to 3, the composition of the cured resin and the process thereof were different from those of example 1; the solder resist obtained in comparative example 4, the composition of the epoxy resin and the process thereof were different from those of comparative example 3; the dielectric constant and the loss factor data are improved, and the peel strength data are reduced; it can be known that the dielectric property and the bonding property of the solder mask are improved by setting the components and the process in the cured resin and the epoxy resin.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Furthermore, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process method article or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process method article or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement and improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A processing technology of a single-sided PCB printed circuit board is characterized in that: the method comprises the following processes:
(1) pretreatment: cutting and cleaning the copper-clad substrate;
(2) preparing a circuit: printing a circuit pattern, carrying out UV drying, etching and film stripping;
(3) solder resist printing: coating solder resist ink and carrying out UV drying;
(3) printing of characters: printing characters on the back and the front of the copper-clad substrate, and performing UV drying;
(5) and (3) post-treatment: drilling and punching a positioning hole;
the solder resist ink comprises the following components in parts by weight: the component A comprises: 40-60 parts of curing resin, 25-45 parts of titanium dioxide, 0-15 parts of barium sulfate, 4-7 parts of photoinitiator and 2-7 parts of auxiliary agent;
And B component: 25-40 parts of epoxy resin, 0-20 parts of titanium dioxide, 2-5 parts of fumed silica, 20-45 parts of diluent, 5-12 parts of auxiliary agent and 15-30 parts of solvent;
the cured resin is prepared by the following process:
1.1. mixing dicyclopentadiene and aluminum chloride, heating to 120-130 ℃ in a nitrogen atmosphere, and preserving heat for 1.6-2.5 h; slowly adding divinylbenzene, and reacting for 3.6-4.5 hours under heat preservation; adding a 5% sodium hydroxide solution, stirring for 50-75 min, filtering and washing; distilling the organic phase; dissolving toluene, extracting with deionized water, repeating for many times, and distilling to obtain dicyclopentadiene derivative A;
1.2. taking 2, 2-bis [ (3-amido-4-hydroxyl) phenyl]Hexafluoropropane, Et3N, Sm (OTf) 3 Mixing, adding an ethanol water solution, slowly adding 4-vinylbenzaldehyde at the temperature of 75-85 ℃ in a nitrogen atmosphere, and carrying out reflux reaction for 10-15 h; adding deionized water after reaction, and performing suction filtration to obtain a benzothiazole derivative B;
1.3. heating acetone to 80-100 ℃ in a nitrogen atmosphere; slowly dropwise adding a mixed monomer of the dicyclopentadiene derivative A, the benzothiazole derivative B, the initiator and the chain transfer agent, and finishing dropwise adding for 2-3 h; reacting for 2-4 h at the temperature of 85-100 ℃ in a heat preservation manner; heating to 95-115 ℃, and reacting for 1-2 h; and heating to 115-125 ℃, and continuing to react for 60-90 min for 1-2 h to obtain the cured resin.
2. The process for manufacturing a single-sided PCB printed wiring board according to claim 1, wherein: the molar ratio of the divinylbenzene to the aluminum chloride to the dicyclopentadiene to the sodium hydroxide solution is 1 (0.020-0.022) to 0.013-0.015) to 0.083-0.085;
the 2, 2-bis [ (3-amino-4-hydroxy) phenyl group]Hexafluoropropane, 4-vinylbenzaldehyde, Et3N, Sm (OTf) 3 The molar ratio of (1), (1.2-1.5), (1.6-E)2.0):(0.16～0.20)。
3. The process for manufacturing a single-sided PCB printed wiring board according to claim 1, wherein: the mass ratio of the acetone, the dicyclopentadiene derivative A, the benzothiazole derivative B, the initiator and the chain transfer agent is (41-67): (20-45): (15-35): (0.5-3.0): (0.1-0.5).
4. The process for manufacturing a single-sided PCB printed wiring board according to claim 1, wherein: the epoxy resin is prepared by the following process:
2.1. mixing 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone and toluene, adding trifluoromethanesulfonic acid, stirring, and reacting for 72 h; pouring into ice water, separating an organic phase, washing by using 5% sodium bicarbonate water solution and distilled water, distilling, and recrystallizing and purifying by using petroleum ether to obtain a dimethyl product A;
Mixing the product A, pyridine and distilled water, heating and refluxing, and reacting for 3-4 h; adding potassium permanganate, and stirring and reacting for 2.7-3.2 h; filtering, concentrating, adding a sodium hydroxide aqueous solution, and heating and refluxing for 2-4 h; adding potassium permanganate again, and refluxing for 2.7-3.2 h; cooling to 60-72 ℃, slowly adding ethanol, and refluxing for 50-70 min; filtering, concentrating, adjusting the pH to 1-2 by using dilute hydrochloric acid, filtering, washing by using dilute hydrochloric acid salt and distilled water, and drying in vacuum to obtain a diacid product B;
mixing the diacid product B, thionyl chloride and N, N-dimethylformamide, stirring and refluxing for 5.6-6.4 h, carrying out vacuum distillation, cooling, filtering, and recrystallizing and purifying anhydrous petroleum ether to obtain a diacyl chloride product C;
2.2. taking toluene, adding a diacyl chloride product C, 1,3, 5-tri (2-hydroxyethyl) -1,3, 5-triazine-2, 4, 6-trione and p-toluenesulfonic acid, heating to reflux under the protection of nitrogen, and reacting for 3-4 h; cooling to room temperature, washing with 5% sodium bicarbonate water solution and distilled water, drying the organic layer, filtering, and rotary evaporating to obtain ester D;
2.3. dissolving glycidol in benzene, adding triethylamine, adjusting the temperature of the system to 0 ℃, slowly adding the esterified substance D, stirring for 4-5 h, and standing for 20-24 h at room temperature; filtering, concentrating, washing with 5% sodium bicarbonate ice water solution and distilled water, and drying to obtain the epoxy resin.
5. The process for manufacturing a single-sided PCB printed wiring board according to claim 4, wherein: the molar ratio of the 3-trifluoromethyl-2, 2, 2-trifluoro acetophenone to the toluene to the trifluoromethanesulfonic acid is 1:8: 0.8;
the molar ratio of the product A, pyridine to potassium permanganate to be added again to sodium hydroxide is 1 (51-52) to 6:5 (14.0-14.4);
the molar ratio of the diacid product B to the thionyl chloride is 1 (45-47).
6. The process for manufacturing a single-sided PCB printed wiring board according to claim 4, wherein: the mole ratio of the diacyl chloride product C, 1,3, 5-tri (2-hydroxyethyl) -1,3, 5-triazine-2, 4, 6-trione and p-toluenesulfonic acid is (3.05-3.10) to 1 (0.023-0.046).
7. The process for manufacturing a single-sided PCB printed wiring board according to claim 4, wherein: the molar ratio of the glycidol to the triethylamine to the ester D is (2.2-2.4): 2.1-2.3): 1.
8. A single-sided PCB printed wiring board made according to the process of any one of claims 1 to 7.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2013194057A (en) * | 2012-03-15 | 2013-09-30 | Sanwa Kagaku Kogyo Kk | Composition for forming solder resist for led |
| CN106132098A (en) * | 2016-06-30 | 2016-11-16 | 浙江罗奇泰克电子有限公司 | A kind of manufacture method of LED metal base circuit board |
| CN107722713A (en) * | 2017-10-09 | 2018-02-23 | 广东高仕电研科技有限公司 | Two-component liquid photosensitive white solder mask for PCB and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013194057A (en) * | 2012-03-15 | 2013-09-30 | Sanwa Kagaku Kogyo Kk | Composition for forming solder resist for led |
| CN106132098A (en) * | 2016-06-30 | 2016-11-16 | 浙江罗奇泰克电子有限公司 | A kind of manufacture method of LED metal base circuit board |
| CN107722713A (en) * | 2017-10-09 | 2018-02-23 | 广东高仕电研科技有限公司 | Two-component liquid photosensitive white solder mask for PCB and preparation method thereof |
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