CN116075068A - Cleaning and antioxidation process for preventing copper surface from oxidization based on copper foil of printed circuit board - Google Patents
Cleaning and antioxidation process for preventing copper surface from oxidization based on copper foil of printed circuit board Download PDFInfo
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- CN116075068A CN116075068A CN202211682012.8A CN202211682012A CN116075068A CN 116075068 A CN116075068 A CN 116075068A CN 202211682012 A CN202211682012 A CN 202211682012A CN 116075068 A CN116075068 A CN 116075068A
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- circuit board
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- antioxidation
- washing
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- 230000003064 anti-oxidating effect Effects 0.000 title claims abstract description 76
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 31
- 239000010949 copper Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000004140 cleaning Methods 0.000 title claims abstract description 27
- 239000011889 copper foil Substances 0.000 title claims abstract description 27
- 238000007254 oxidation reaction Methods 0.000 title claims description 36
- 238000005507 spraying Methods 0.000 claims abstract description 56
- 239000011241 protective layer Substances 0.000 claims abstract description 29
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 21
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 21
- 239000010410 layer Substances 0.000 claims abstract description 20
- 238000005516 engineering process Methods 0.000 claims abstract description 19
- 239000003463 adsorbent Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims description 107
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 60
- 238000001035 drying Methods 0.000 claims description 50
- 230000003647 oxidation Effects 0.000 claims description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000003963 antioxidant agent Substances 0.000 claims description 26
- 230000003078 antioxidant effect Effects 0.000 claims description 26
- 230000002745 absorbent Effects 0.000 claims description 25
- 239000002250 absorbent Substances 0.000 claims description 25
- 239000003921 oil Substances 0.000 claims description 23
- 239000007788 liquid Substances 0.000 claims description 20
- 238000005554 pickling Methods 0.000 claims description 20
- 238000005238 degreasing Methods 0.000 claims description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 18
- 239000012153 distilled water Substances 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 18
- 239000008399 tap water Substances 0.000 claims description 18
- 235000020679 tap water Nutrition 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 16
- 238000013007 heat curing Methods 0.000 claims description 16
- BAERPNBPLZWCES-UHFFFAOYSA-N (2-hydroxy-1-phosphonoethyl)phosphonic acid Chemical compound OCC(P(O)(O)=O)P(O)(O)=O BAERPNBPLZWCES-UHFFFAOYSA-N 0.000 claims description 10
- IXDGHAZCSMVIFX-UHFFFAOYSA-N 6-(dibutylamino)-1h-1,3,5-triazine-2,4-dithione Chemical compound CCCCN(CCCC)C1=NC(=S)NC(=S)N1 IXDGHAZCSMVIFX-UHFFFAOYSA-N 0.000 claims description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 10
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 10
- 239000012964 benzotriazole Substances 0.000 claims description 10
- 239000013527 degreasing agent Substances 0.000 claims description 10
- 238000005237 degreasing agent Methods 0.000 claims description 10
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 claims description 10
- 229940043264 dodecyl sulfate Drugs 0.000 claims description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 10
- 239000000080 wetting agent Substances 0.000 claims description 10
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 8
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 8
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 8
- 235000012207 sodium gluconate Nutrition 0.000 claims description 8
- 239000000176 sodium gluconate Substances 0.000 claims description 8
- 229940005574 sodium gluconate Drugs 0.000 claims description 8
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 8
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 8
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 8
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 7
- 239000004519 grease Substances 0.000 claims description 3
- 238000010301 surface-oxidation reaction Methods 0.000 claims 2
- 239000006096 absorbing agent Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 14
- 238000004649 discoloration prevention Methods 0.000 abstract description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 3
- 230000032683 aging Effects 0.000 abstract description 2
- 230000002265 prevention Effects 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- 239000007921 spray Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 9
- 230000007797 corrosion Effects 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004381 surface treatment Methods 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000004699 copper complex Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
Images
Classifications
-
- 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
- H05K3/22—Secondary treatment of printed circuits
- H05K3/26—Cleaning or polishing of the conductive pattern
-
- 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
- H05K3/22—Secondary treatment of printed circuits
- H05K3/227—Drying of printed circuits
-
- 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
- H05K3/22—Secondary treatment of printed circuits
- H05K3/28—Applying non-metallic protective coatings
-
- 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
- H05K3/22—Secondary treatment of printed circuits
- H05K3/28—Applying non-metallic protective coatings
- H05K3/282—Applying non-metallic protective coatings for inhibiting the corrosion of the circuit, e.g. for preserving the solderability
Landscapes
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing Of Printed Wiring (AREA)
Abstract
The invention discloses a cleaning and antioxidation process for preventing copper surfaces from being oxidized based on a copper foil of a printed circuit board. The invention can perform antioxidation protection on the surface of the circuit board, thereby improving the antioxidation capability of the circuit board, in addition, by utilizing the nano spraying technology to spray an antioxidation adsorbent on the surface of the circuit board, the adsorption effect of the antioxidation layer can be effectively improved, and simultaneously, by spraying the nano silicon oxide protective layer on the surface of the antioxidation layer, the antioxidation layer can be protected, thereby effectively prolonging the protection aging of the antioxidation layer, and the circuit board after the antioxidation treatment has the advantages of good discoloration prevention effect, good rust prevention effect and good antioxidation effect, and effectively prolonging the service life of the circuit board.
Description
Technical Field
The invention relates to the technical field of metal surface treatment, in particular to a cleaning and antioxidation process for preventing copper surfaces from being oxidized based on copper foils of printed circuit boards.
Background
With the development of economy, electronic products are being developed in the directions of light weight, thin thickness, short length, miniaturization and multifunction, so that circuit boards are being developed in the directions of high precision, thin thickness, multilayering and small holes. Copper on the surface of the circuit board is usually treated with oxygen-containing water, oxidizing acid and CN - 、NH4 + Complex ions can be formed in the solution to generate serious corrosion, and the corrosion resistance is poor in a humid atmosphere and a strong corrosion medium containing an oxidant, so that the service life of the circuit board is easy to be directly influenced.
Along with the development of circuit board technology, the circuit board has increased the oxidation resistance process in the production process adaptability, and the chemical method is used to generate a brown involucra of organic copper complex on the bare braze welding surface after preventing welding, so that the surface of the circuit board has an oxidation resistance protective film layer. However, the surface treatment of the copper foil of the printed circuit board manufactured by the traditional antioxidation process has the defects of poor discoloration prevention effect, poor antioxidation effect, easy insulation and short service life, so that the antioxidation process with good discoloration prevention effect, good rust prevention effect and good antioxidation effect is found to have important significance.
For the problems in the related art, no effective solution has been proposed at present.
Disclosure of Invention
Aiming at the problems in the related art, the invention provides a cleaning and antioxidation process for preventing copper surfaces from being oxidized based on copper foils of a printed circuit board so as to overcome the technical problems in the prior art.
For this purpose, the invention adopts the following specific technical scheme:
a cleaning and antioxidation process for preventing copper surfaces from being oxidized based on copper foil of a printed circuit board comprises the following steps:
s1, degreasing, namely immersing a circuit board to be treated in a degreasing agent for degreasing treatment;
s2, washing the circuit board subjected to oil removal by using tap water;
s3, microetching, namely immersing the circuit board after water washing in a microetching solution to perform microetching treatment;
s4, washing again, and washing the circuit board subjected to microetching again by using tap water;
s5, pickling, namely immersing the circuit board subjected to the secondary washing in sulfuric acid for pickling treatment;
s6, washing and drying, namely repeatedly washing the pickled circuit board by using distilled water, and drying by using compressed air;
s7, spraying an adsorbent, namely spraying a layer of antioxidant absorbent on the surface of the washed and dried circuit board by a nano spraying technology;
s8, performing antioxidation treatment, namely immersing the circuit board sprayed with the antioxidation absorbent in the antioxidation liquid for performing the antioxidation treatment;
s9, washing and drying again, repeatedly washing the circuit board subjected to the antioxidation treatment by using distilled water again, and drying by using compressed air;
s10, spraying a protective layer, namely spraying a nano silicon oxide protective layer on the surface of the circuit board after washing and drying again by using a nano spraying technology;
s11, performing heat curing treatment on the circuit board sprayed with the nano silicon oxide protective layer by using a far infrared heating lamp.
Further, the oil removing agent comprises the following raw materials in parts by weight:
5-10 parts of sodium dodecyl benzene sulfonate, 1-3 parts of butanol, 2-5 parts of sodium pyrophosphate, 1-2 parts of sodium tripolyphosphate, 1-2 parts of saponified grease, 2-5 parts of sodium gluconate and 100-150 parts of water.
Further, the temperature of the oil removal treatment is 30-35 ℃, and the treatment time is 30-45 seconds.
Further, the temperature of the water washing treatment, the water washing treatment again and the acid washing treatment are all room temperature, the time of the water washing treatment is 35-55 seconds, the time of the water washing treatment again is 25-35 seconds, and the time of the acid washing treatment is 30-50 seconds.
Further, the temperature of the microetching treatment is 25-30 ℃, and the time of the microetching treatment is 40-55 seconds.
Further, the time of the flushing and drying and the time of the re-flushing and drying are both 50-65 seconds, the compressed air is normal-temperature compressed air, and the included angle between the air outlet direction of the compressed air and the plane of the circuit board is 10-40 degrees.
Further, the spraying thickness of the antioxidant absorbent and the nano silicon oxide protective layer is 0.01-0.02 microns.
Further, the time of the antioxidation treatment is 60-100 seconds, and the temperature of the antioxidation treatment is 30-45 ℃.
Further, the antioxidant liquid consists of the following raw materials in parts by weight:
5-10 parts of hydroxyethylidene diphosphonic acid, 3-8 parts of di-p-chlorobenzyl benzimidazole, 1-5 parts of benzotriazole, 1-3 parts of sodium hydroxide, 5-10 parts of ethanol, 1-5 parts of dodecyl sulfate, 3-5 parts of polyvinyl alcohol, 1-3 parts of 6- (dibutylamino) -1,3, 5-triazine-2, 4-dithiol, 1-3 parts of wetting agent and 100-150 parts of water.
Further, the temperature of the heat curing treatment is 70-85 ℃, and the time of the heat curing treatment is 10-30 seconds.
The beneficial effects of the invention are as follows:
1) The oxidation-resistant layer is formed on the copper surface of the circuit board in a dipping mode, so that the surface of the circuit board can be subjected to oxidation-resistant protection, the oxidation-resistant capability of the circuit board can be improved, in addition, the adsorption effect of the oxidation-resistant layer can be effectively improved by spraying the oxidation-resistant adsorbent on the surface of the circuit board by utilizing a nano spraying technology, and meanwhile, the oxidation-resistant layer can be protected by spraying the nano silicon oxide protective layer on the surface of the oxidation-resistant layer, so that the protection aging of the oxidation-resistant layer can be effectively prolonged, and the circuit board after oxidation resistance treatment has the advantages of good discoloration-resistant effect, good rust-resistant effect and good oxidation-resistant effect, and the service life of the circuit board is effectively prolonged.
2) The raw materials such as hydroxyethylidene diphosphonic acid, di-p-chlorobenzyl benzimidazole, benzotriazole, sodium hydroxide, dodecyl sulfate, polyvinyl alcohol, 6- (dibutylamino) -1,3, 5-triazine-2, 4-dithiol, wetting agent and the like are matched for use, so that the stability, corrosion resistance, high temperature resistance and oxidation resistance of the antioxidant liquid can be effectively improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a cleaning and oxidation resistant process for preventing oxidation of copper surfaces based on a copper foil of a printed circuit board according to an embodiment of the present invention;
fig. 2 is a schematic diagram showing the results of the thermal stability test of examples 1 to 5 and comparative example 1 in a cleaning oxidation-resistant process for preventing oxidation of copper surfaces based on copper foil of a printed circuit board according to an embodiment of the present invention.
Detailed Description
For the purpose of further illustrating the various embodiments, the present invention provides the accompanying drawings, which are a part of the disclosure of the present invention, and which are mainly used to illustrate the embodiments and, together with the description, serve to explain the principles of the embodiments, and with reference to these descriptions, one skilled in the art will recognize other possible implementations and advantages of the present invention, wherein elements are not drawn to scale, and like reference numerals are generally used to designate like elements.
According to an embodiment of the invention, a cleaning and antioxidation process for preventing oxidation of a copper surface based on a copper foil of a printed circuit board is provided.
The invention will be further described with reference to the accompanying drawings and detailed description, as shown in fig. 1-2, a cleaning and oxidation-resisting process for preventing oxidation of copper surfaces based on copper foil of a printed circuit board according to an embodiment of the invention, the cleaning and oxidation-resisting process comprising the following steps:
s1, degreasing, namely immersing a circuit board to be treated in a degreasing agent for degreasing treatment;
wherein the temperature of the oil removal treatment is 30-35 ℃ and the treatment time is 30-45 seconds.
Specifically, the oil removing agent consists of the following raw materials in parts by weight:
5-10 parts of sodium dodecyl benzene sulfonate, 1-3 parts of butanol, 2-5 parts of sodium pyrophosphate, 1-2 parts of sodium tripolyphosphate, 1-2 parts of saponified grease, 2-5 parts of sodium gluconate and 100-150 parts of water.
S2, washing the circuit board subjected to oil removal by using tap water;
wherein the temperature of the water washing treatment is room temperature, and the time of the water washing treatment is 35-55 seconds.
S3, microetching, namely immersing the circuit board after water washing in a microetching solution to perform microetching treatment;
wherein the temperature of the microetching treatment is 25-30 ℃, and the time of the microetching treatment is 40-55 seconds.
S4, washing again, and washing the circuit board subjected to microetching again by using tap water;
wherein the temperature of the re-washing treatment is room temperature, and the time of the re-washing treatment is 25-35 seconds.
S5, pickling, namely immersing the circuit board subjected to the secondary washing in sulfuric acid for pickling treatment;
wherein the temperature of the pickling treatment is room temperature, and the pickling treatment time is 30-50 seconds.
S6, washing and drying, namely repeatedly washing the pickled circuit board by using distilled water, and drying by using compressed air;
the washing and drying time is 50-65 seconds, the compressed air is normal-temperature compressed air, and an included angle between the air outlet direction of the compressed air and a plane where the circuit board is located is 10-40 degrees.
S7, spraying an adsorbent, namely spraying a layer of antioxidant absorbent on the surface of the washed and dried circuit board by a nano spraying technology;
wherein the spraying thickness of the antioxidant absorbent is 0.01-0.02 micrometers, and the antioxidant layer absorbent is prepared from butyl acrylate and an adhesive according to the mass ratio of 1:1.5, mixing.
S8, performing antioxidation treatment, namely immersing the circuit board sprayed with the antioxidation absorbent in the antioxidation liquid for performing the antioxidation treatment;
wherein the time of the antioxidation treatment is 60-100 seconds, and the temperature of the antioxidation treatment is 30-45 ℃.
Specifically, the antioxidant liquid consists of the following raw materials in parts by weight:
5-10 parts of hydroxyethylidene diphosphonic acid, 3-8 parts of di-p-chlorobenzyl benzimidazole, 1-5 parts of benzotriazole, 1-3 parts of sodium hydroxide, 5-10 parts of ethanol, 1-5 parts of dodecyl sulfate, 3-5 parts of polyvinyl alcohol, 1-3 parts of 6- (dibutylamino) -1,3, 5-triazine-2, 4-dithiol, 1-3 parts of wetting agent and 100-150 parts of water.
S9, washing and drying again, repeatedly washing the circuit board subjected to the antioxidation treatment by using distilled water again, and drying by using compressed air;
the secondary washing and drying time is 50-65 seconds, the compressed air is normal-temperature compressed air, and an included angle between the air outlet direction of the compressed air and the plane of the circuit board is 10-40 degrees.
S10, spraying a protective layer, namely spraying a nano silicon oxide protective layer on the surface of the circuit board after washing and drying again by using a nano spraying technology;
wherein the spraying thickness of the nano silicon oxide protective layer is 0.01-0.02 micrometers.
S11, performing heat curing treatment on the circuit board sprayed with the nano silicon oxide protective layer by using a far infrared heating lamp.
Wherein the temperature of the heat curing treatment is 70-85 ℃, and the time of the heat curing treatment is 10-30 seconds.
In order to facilitate understanding of the above technical solutions of the present invention, specific embodiments of the present invention are described in detail below.
Example 1
A cleaning and antioxidation process for preventing copper surfaces from being oxidized based on copper foil of a printed circuit board comprises the following steps:
s1, degreasing, namely immersing a circuit board to be treated in a degreasing agent at 30 ℃ for degreasing treatment for 30 seconds;
specifically, the oil removing agent consists of the following raw materials in parts by weight:
5g of sodium dodecyl benzene sulfonate, 1g of butanol, 2g of sodium pyrophosphate, 1g of sodium tripolyphosphate, 1g of saponified oil and fat, 2g of sodium gluconate and 100ml of water.
S2, washing the circuit board subjected to oil removal by using tap water at room temperature for 35 seconds;
s3, microetching, namely immersing the circuit board after water washing in a microetching solution at 25 ℃ for microetching treatment for 40 seconds;
s4, washing again, namely washing the circuit board subjected to microetching again by using tap water at room temperature for 25 seconds;
s5, pickling, namely immersing the circuit board subjected to the water washing again in sulfuric acid at room temperature for pickling for 30 seconds;
s6, washing and drying, namely repeatedly washing the pickled circuit board for 40 seconds by using distilled water, and drying for 10 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and a plane where the circuit board is located is 40 degrees.
S7, spraying an adsorbent, namely spraying a layer of 0.01-micrometer antioxidant absorbent on the surface of the washed and dried circuit board by a nano spraying technology, wherein the antioxidant absorbent is prepared from butyl acrylate and an adhesive according to a mass ratio of 1:1.5, mixing.
S8, performing antioxidation treatment, namely immersing the circuit board sprayed with the antioxidation absorbent in the antioxidation liquid at 30 ℃ for 60 seconds;
the antioxidant liquid consists of the following raw materials in parts by weight:
5 parts of hydroxyethylidene diphosphonic acid, 3 parts of di-p-chlorobenzyl benzimidazole, 1 part of benzotriazole, 1 part of sodium hydroxide, 5 parts of ethanol, 1 part of dodecyl sulfate, 3 parts of polyvinyl alcohol, 1 part of 6- (dibutylamino) -1,3, 5-triazine-2, 4-dithiol, 1 part of wetting agent and 100 parts of water.
S9, washing and drying again, repeatedly washing the circuit board subjected to the antioxidation treatment for 40 seconds by using distilled water again, and drying for 10 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and the plane of the circuit board is 40 degrees.
S10, spraying a protective layer, namely spraying a nano silicon oxide protective layer with the thickness of 0.01 micrometer on the surface of the circuit board after washing and drying again by using a nano spraying technology;
s11, heat curing, namely performing heat curing treatment on the circuit board sprayed with the nano silicon oxide protective layer for 10 seconds by using a far infrared heating lamp at 70 ℃.
Example 2
A cleaning and antioxidation process for preventing copper surfaces from being oxidized based on copper foil of a printed circuit board comprises the following steps:
s1, degreasing, namely immersing a circuit board to be treated in a degreasing agent at 30 ℃ for degreasing treatment for 35 seconds;
specifically, the oil removing agent consists of the following raw materials in parts by weight:
6g of sodium dodecyl benzene sulfonate, 1g of butanol, 2g of sodium pyrophosphate, 1g of sodium tripolyphosphate, 1g of saponified oil and fat, 2g of sodium gluconate and 110ml of water.
S2, washing the circuit board subjected to oil removal by using tap water at room temperature for 40 seconds;
s3, microetching, namely immersing the circuit board after water washing in a microetching solution at 25 ℃ for microetching treatment for 40 seconds;
s4, washing again, namely washing the circuit board subjected to microetching again by using tap water at room temperature for 30 seconds;
s5, pickling, namely immersing the circuit board subjected to the water washing again in sulfuric acid at room temperature for pickling for 35 seconds;
s6, washing and drying, namely repeatedly washing the pickled circuit board for 45 seconds by using distilled water, and drying for 15 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and a plane where the circuit board is located is 35 degrees.
S7, spraying an adsorbent, namely spraying a layer of 0.01-micrometer antioxidant absorbent on the surface of the washed and dried circuit board by a nano spraying technology, wherein the antioxidant absorbent is prepared from butyl acrylate and an adhesive according to a mass ratio of 1:1.5, mixing.
S8, performing antioxidation treatment, namely immersing the circuit board sprayed with the antioxidation absorbent in the antioxidation liquid at 30 ℃ for 70 seconds;
the antioxidant liquid consists of the following raw materials in parts by weight:
6 parts of hydroxyethylidene diphosphonic acid, 3 parts of di-p-chlorobenzyl benzimidazole, 1 part of benzotriazole, 1 part of sodium hydroxide, 5 parts of ethanol, 1 part of dodecyl sulfate, 3 parts of polyvinyl alcohol, 1 part of 6- (dibutylamino) -1,3, 5-triazine-2, 4-dithiol, 1 part of wetting agent and 110 parts of water.
S9, washing and drying again, repeatedly washing the circuit board subjected to the antioxidation treatment for 45 seconds by using distilled water again, and drying for 15 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and a plane where the circuit board is located is 35 degrees.
S10, spraying a protective layer, namely spraying a nano silicon oxide protective layer with the thickness of 0.01 micrometer on the surface of the circuit board after washing and drying again by using a nano spraying technology;
s11, heat curing, namely performing heat curing treatment on the circuit board sprayed with the nano silicon oxide protective layer for 15 seconds by using a far infrared heating lamp at 70 ℃.
Example 3
A cleaning and antioxidation process for preventing copper surfaces from being oxidized based on copper foil of a printed circuit board comprises the following steps:
s1, degreasing, namely immersing a circuit board to be treated in a degreasing agent at 35 ℃ for degreasing treatment for 30 seconds;
specifically, the oil removing agent consists of the following raw materials in parts by weight:
7g of sodium dodecyl benzene sulfonate, 1g of butanol, 2g of sodium pyrophosphate, 1g of sodium tripolyphosphate, 1g of saponified oil and fat, 2g of sodium gluconate and 120ml of water.
S2, washing the circuit board subjected to oil removal by using tap water at room temperature for 35 seconds;
s3, microetching, namely immersing the circuit board after water washing in a microetching solution at 30 ℃ for microetching treatment for 40 seconds;
s4, washing again, namely washing the circuit board subjected to microetching again by using tap water at room temperature for 25 seconds;
s5, pickling, namely immersing the circuit board subjected to the water washing again in sulfuric acid at room temperature for pickling for 30 seconds;
s6, washing and drying, namely repeatedly washing the pickled circuit board for 40 seconds by using distilled water, and drying for 10 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and a plane where the circuit board is located is 10 degrees.
S7, spraying an adsorbent, namely spraying a layer of 0.01-micrometer antioxidant absorbent on the surface of the washed and dried circuit board by a nano spraying technology, wherein the antioxidant absorbent is prepared from butyl acrylate and an adhesive according to a mass ratio of 1:1.5, mixing.
S8, performing antioxidation treatment, namely immersing the circuit board sprayed with the antioxidation absorbent in the antioxidation liquid at 35 ℃ for 60 seconds;
the antioxidant liquid consists of the following raw materials in parts by weight:
7 parts of hydroxyethylidene diphosphonic acid, 3 parts of di-p-chlorobenzyl benzimidazole, 1 part of benzotriazole, 1 part of sodium hydroxide, 5 parts of ethanol, 1 part of dodecyl sulfate, 3 parts of polyvinyl alcohol, 1 part of 6- (dibutylamino) -1,3, 5-triazine-2, 4-dithiol, 1 part of wetting agent and 120 parts of water.
S9, washing and drying again, repeatedly washing the circuit board subjected to the antioxidation treatment for 40 seconds by using distilled water again, and drying for 10 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and the plane of the circuit board is 40 degrees.
S10, spraying a protective layer, namely spraying a nano silicon oxide protective layer with the thickness of 0.01 micrometer on the surface of the circuit board after washing and drying again by using a nano spraying technology;
s11, performing heat curing treatment on the circuit board sprayed with the nano silicon oxide protective layer for 10 seconds by using a far infrared heating lamp at 75 ℃.
Example 4
A cleaning and antioxidation process for preventing copper surfaces from being oxidized based on copper foil of a printed circuit board comprises the following steps:
s1, degreasing, namely immersing a circuit board to be treated in a degreasing agent at 35 ℃ for degreasing treatment for 35 seconds;
specifically, the oil removing agent consists of the following raw materials in parts by weight:
9g of sodium dodecyl benzene sulfonate, 1g of butanol, 2g of sodium pyrophosphate, 1g of sodium tripolyphosphate, 1g of saponified oil and fat, 2g of sodium gluconate and 140ml of water.
S2, washing the circuit board subjected to oil removal by using tap water at room temperature for 40 seconds;
s3, microetching, namely immersing the circuit board after water washing in a microetching solution at 30 ℃ for microetching treatment for 45 seconds;
s4, washing again, namely washing the circuit board subjected to microetching again by using tap water at room temperature for 30 seconds;
s5, pickling, namely immersing the circuit board subjected to the water washing again in sulfuric acid at room temperature for pickling for 35 seconds;
s6, washing and drying, namely repeatedly washing the pickled circuit board for 45 seconds by using distilled water, and drying for 15 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and a plane where the circuit board is located is 35 degrees.
S7, spraying an adsorbent, namely spraying a layer of 0.01-micrometer antioxidant absorbent on the surface of the washed and dried circuit board by a nano spraying technology, wherein the antioxidant absorbent is prepared from butyl acrylate and an adhesive according to a mass ratio of 1:1.5, mixing.
S8, performing antioxidation treatment, namely immersing the circuit board sprayed with the antioxidation absorbent in the antioxidation liquid at 35 ℃ for 70 seconds;
the antioxidant liquid consists of the following raw materials in parts by weight:
9 parts of hydroxyethylidene diphosphonic acid, 3 parts of di-p-chlorobenzyl benzimidazole, 1 part of benzotriazole, 1 part of sodium hydroxide, 5 parts of ethanol, 1 part of dodecyl sulfate, 3 parts of polyvinyl alcohol, 1 part of 6- (dibutylamino) -1,3, 5-triazine-2, 4-dithiol, 1 part of wetting agent and 140 parts of water.
S9, washing and drying again, repeatedly washing the circuit board subjected to the antioxidation treatment for 45 seconds by using distilled water again, and drying for 15 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and a plane where the circuit board is located is 35 degrees.
S10, spraying a protective layer, namely spraying a nano silicon oxide protective layer with the thickness of 0.01 micrometer on the surface of the circuit board after washing and drying again by using a nano spraying technology;
s11, performing heat curing treatment on the circuit board sprayed with the nano silicon oxide protective layer for 15 seconds by using a far infrared heating lamp at 75 ℃.
Example 5
A cleaning and antioxidation process for preventing copper surfaces from being oxidized based on copper foil of a printed circuit board comprises the following steps:
s1, degreasing, namely immersing a circuit board to be treated in a degreasing agent at 35 ℃ for degreasing treatment for 45 seconds;
specifically, the oil removing agent consists of the following raw materials in parts by weight:
10g of sodium dodecyl benzene sulfonate, 3g of butanol, 5g of sodium pyrophosphate, 2g of sodium tripolyphosphate, 2g of saponified oil and fat, 5g of sodium gluconate and 150ml of water.
S2, washing the circuit board subjected to oil removal by using tap water at room temperature for 55 seconds;
s3, microetching, namely immersing the circuit board after water washing in a microetching solution at 30 ℃ for microetching treatment for 55 seconds;
s4, washing again, and washing the circuit board subjected to microetching again by using tap water at room temperature for 35 seconds;
s5, pickling, namely immersing the circuit board subjected to the water washing again in sulfuric acid at room temperature for pickling for 50 seconds;
s6, washing and drying, namely repeatedly washing the pickled circuit board for 50 seconds by using distilled water, and drying for 15 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and a plane where the circuit board is located is 10 degrees.
S7, spraying an adsorbent, namely spraying a layer of 0.02-micrometer antioxidant absorbent on the surface of the washed and dried circuit board by a nano spraying technology, wherein the antioxidant absorbent is prepared from butyl acrylate and an adhesive according to a mass ratio of 1:1.5, mixing.
S8, performing antioxidation treatment, namely immersing the circuit board sprayed with the antioxidation absorbent in the antioxidation liquid at 30 ℃ for 100 seconds;
the antioxidant liquid consists of the following raw materials in parts by weight:
10 parts of hydroxyethylidene diphosphonic acid, 8 parts of di-p-chlorobenzyl benzimidazole, 5 parts of benzotriazole, 3 parts of sodium hydroxide, 10 parts of ethanol, 5 parts of dodecyl sulfate, 5 parts of polyvinyl alcohol, 3 parts of 6- (dibutylamino) -1,3, 5-triazine-2, 4-dithiol, 3 parts of a wetting agent and 150 parts of water.
S9, washing and drying again, repeatedly washing the circuit board subjected to the antioxidation treatment for 50 seconds by using distilled water again, and drying for 15 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and a plane where the circuit board is located is 10 degrees.
S10, spraying a protective layer, namely spraying a nano silicon oxide protective layer with the thickness of 0.02 microns on the surface of the circuit board after washing and drying again by using a nano spraying technology;
s11, performing heat curing treatment on the circuit board sprayed with the nano silicon oxide protective layer for 30 seconds by using a far infrared heating lamp at the temperature of 85 ℃.
Comparative example 1
A cleaning and antioxidation process for preventing copper surfaces from being oxidized based on copper foil of a printed circuit board comprises the following steps:
s1, degreasing, namely immersing a circuit board to be treated in a degreasing agent (purchased in the market) at 30 ℃ for degreasing treatment for 30 seconds;
s2, washing the circuit board subjected to oil removal by using tap water at room temperature for 35 seconds;
s3, microetching, namely immersing the circuit board after water washing in a microetching solution at 25 ℃ for microetching treatment for 40 seconds;
s4, washing again, namely washing the circuit board subjected to microetching again by using tap water at room temperature for 25 seconds;
s5, pickling, namely immersing the circuit board subjected to the water washing again in sulfuric acid at room temperature for pickling for 30 seconds;
s6, washing and drying, namely repeatedly washing the pickled circuit board for 40 seconds by using distilled water, and drying for 10 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and a plane where the circuit board is located is 40 degrees.
S7, performing antioxidation treatment, namely immersing the circuit board sprayed with the antioxidation absorbent in an antioxidation liquid (conventional antioxidation liquid on the market) at 30 ℃ for 60 seconds;
and S8, washing and drying again, repeatedly washing the circuit board subjected to the antioxidation treatment for 40 seconds by using distilled water again, and drying for 10 seconds by using normal-temperature compressed air, wherein an included angle between the air outlet direction of the compressed air and the plane of the circuit board is 40 degrees.
Experimental example
The circuit boards obtained in examples 1 to 5 and comparative example 1 were subjected to the following performance tests:
high temperature antioxidant test:
the circuit board surfaces of examples 1 to 5 and comparative example 1 were observed and recorded, respectively, for the presence or absence of black oxide substances at high temperatures, and the results are shown in Table 1.
And (3) anti-oxidation test:
the circuit boards of examples 1-5 and comparative example 1 were placed on a dryer separator (note that holes were not blocked), a dryer cover was closed, and placed in an incubator at 35.+ -. 2 ℃ for 72 hours, and the oxidation of the surface of the circuit board was observed and recorded, and the results are shown in Table 1.
Acid corrosion resistance test:
5 drops of hydrochloric acid with the concentration of 0.5mol/L are dripped on the surfaces of the circuit boards of the examples 1-5 and the comparative example 1 according to a plum blossom format, the circuit boards are placed in an environment with the temperature of 200+/-5 ℃ for 5 minutes, and the corrosion condition of the copper surface at the position where the hydrochloric acid is dripped at the 5 positions is observed and recorded, and the result is shown in Table 1.
Thermal stability:
the circuit boards of examples 1-5 and comparative example 1 were left for 7 days, the surface was not discolored, the copper film of the circuit board was scraped off, and the thermal stability was measured using a TA2100 thermogravimetric analyzer, and the results are shown in table 1;
table 1 table of experimental results
As can be seen from the above table analysis, the comparison of the present examples 1 to 5 with comparative example 1 shows that the effects of high temperature oxidation resistance, low temperature oxidation resistance, acid corrosion resistance and thermal stability of examples 1 to 5 are superior to those of comparative example.
In summary, by means of the above technical scheme, the oxidation-resistant layer is formed on the copper surface of the circuit board by adopting the dipping method, so that the oxidation-resistant protection can be performed on the surface of the circuit board, and the oxidation-resistant capability of the circuit board can be improved.
In addition, the stability, the corrosion resistance, the high temperature resistance and the oxidation resistance of the antioxidant liquid can be effectively improved by the combination of raw materials such as hydroxyethylidene diphosphonic acid, di-p-chlorobenzyl benzimidazole, benzotriazole, sodium hydroxide, dodecyl sulfate, polyvinyl alcohol, 6- (dibutylamino) -1,3, 5-triazine-2, 4-dithiol, a wetting agent and the like.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. The cleaning and antioxidation process for preventing the copper surface from being oxidized based on the copper foil of the printed circuit board is characterized by comprising the following steps of:
s1, degreasing, namely immersing a circuit board to be treated in a degreasing agent for degreasing treatment;
s2, washing the circuit board subjected to oil removal by using tap water;
s3, microetching, namely immersing the circuit board after water washing in a microetching solution to perform microetching treatment;
s4, washing again, and washing the circuit board subjected to microetching again by using tap water;
s5, pickling, namely immersing the circuit board subjected to the secondary washing in sulfuric acid for pickling treatment;
s6, washing and drying, namely repeatedly washing the pickled circuit board by using distilled water, and drying by using compressed air;
s7, spraying an adsorbent, namely spraying a layer of antioxidant absorbent on the surface of the washed and dried circuit board by a nano spraying technology;
s8, performing antioxidation treatment, namely immersing the circuit board sprayed with the antioxidation absorbent in the antioxidation liquid for performing the antioxidation treatment;
s9, washing and drying again, repeatedly washing the circuit board subjected to the antioxidation treatment by using distilled water again, and drying by using compressed air;
s10, spraying a protective layer, namely spraying a nano silicon oxide protective layer on the surface of the circuit board after washing and drying again by using a nano spraying technology;
s11, performing heat curing treatment on the circuit board sprayed with the nano silicon oxide protective layer by using a far infrared heating lamp.
2. The cleaning and antioxidation process for preventing copper surfaces from being oxidized based on the copper foil of the printed circuit board according to claim 1, wherein the degreasing agent is composed of the following raw materials in parts by weight:
5-10 parts of sodium dodecyl benzene sulfonate, 1-3 parts of butanol, 2-5 parts of sodium pyrophosphate, 1-2 parts of sodium tripolyphosphate, 1-2 parts of saponified grease, 2-5 parts of sodium gluconate and 100-150 parts of water.
3. The process for cleaning and resisting oxidation based on the copper foil of the printed circuit board to prevent oxidation of copper surfaces according to claim 1, wherein the temperature of the degreasing treatment is 30-35 ℃ and the treatment time is 30-45 seconds.
4. The process for cleaning and resisting oxidation based on copper foil of printed circuit board to prevent oxidation of copper surface according to claim 1, wherein the temperature of the water washing treatment, the re-water washing treatment and the acid washing treatment is room temperature, the time of the water washing treatment is 35-55 seconds, the time of the re-water washing treatment is 25-35 seconds, and the time of the acid washing treatment is 30-50 seconds.
5. The process for cleaning and resisting oxidation based on copper foil of printed circuit board to prevent oxidation of copper surface according to claim 1, wherein the temperature of microetching treatment is 25-30 ℃ and the time of microetching treatment is 40-55 seconds.
6. The process for cleaning and resisting oxidation based on copper foil of printed circuit board to prevent copper surface oxidation according to claim 1, wherein the time for rinsing and drying and the time for rinsing and drying again are both 50-65 seconds, the compressed air is normal-temperature compressed air, and the included angle between the air outlet direction of the compressed air and the plane of the circuit board is 10-40 degrees.
7. The process for cleaning and oxidation preventing copper surface oxidation based on copper foil of printed circuit board according to claim 1, wherein the thickness of the anti-oxidation absorber and the nano silicon oxide protective layer is 0.01-0.02 μm.
8. The process for cleaning and oxidation-preventing copper surfaces based on copper foil for printed circuit boards according to claim 1, wherein the time of the oxidation-preventing treatment is 60-100 seconds, and the temperature of the oxidation-preventing treatment is 30-45 ℃.
9. The cleaning and antioxidation process for preventing copper surfaces from being oxidized based on the copper foil of the printed circuit board according to claim 1, wherein the antioxidation liquid is composed of the following raw materials in parts by weight:
5-10 parts of hydroxyethylidene diphosphonic acid, 3-8 parts of di-p-chlorobenzyl benzimidazole, 1-5 parts of benzotriazole, 1-3 parts of sodium hydroxide, 5-10 parts of ethanol, 1-5 parts of dodecyl sulfate, 3-5 parts of polyvinyl alcohol, 1-3 parts of 6- (dibutylamino) -1,3, 5-triazine-2, 4-dithiol, 1-3 parts of wetting agent and 100-150 parts of water.
10. The process for cleaning and oxidation-preventing copper surfaces based on copper foil for printed circuit boards according to claim 1, wherein the temperature of the heat-curing treatment is 70-85 ℃ and the time of the heat-curing treatment is 10-30 seconds.
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