CN115125526A - Method for chemically plating copper on surface of glass - Google Patents
Method for chemically plating copper on surface of glass Download PDFInfo
- Publication number
- CN115125526A CN115125526A CN202210850368.1A CN202210850368A CN115125526A CN 115125526 A CN115125526 A CN 115125526A CN 202210850368 A CN202210850368 A CN 202210850368A CN 115125526 A CN115125526 A CN 115125526A
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- Prior art keywords
- glass
- treatment
- soaking
- copper plating
- solution
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- 239000011521 glass Substances 0.000 title claims abstract description 167
- 238000007747 plating Methods 0.000 title claims abstract description 105
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000010949 copper Substances 0.000 title claims abstract description 75
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 54
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000126 substance Substances 0.000 claims abstract description 47
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 32
- 230000003213 activating effect Effects 0.000 claims abstract description 17
- 238000007598 dipping method Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 63
- 238000002791 soaking Methods 0.000 claims description 49
- 239000008367 deionised water Substances 0.000 claims description 44
- 229910021641 deionized water Inorganic materials 0.000 claims description 44
- 238000004140 cleaning Methods 0.000 claims description 41
- 230000003750 conditioning effect Effects 0.000 claims description 20
- 230000004913 activation Effects 0.000 claims description 14
- 230000009467 reduction Effects 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008139 complexing agent Substances 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- ZNBNBTIDJSKEAM-UHFFFAOYSA-N 4-[7-hydroxy-2-[5-[5-[6-hydroxy-6-(hydroxymethyl)-3,5-dimethyloxan-2-yl]-3-methyloxolan-2-yl]-5-methyloxolan-2-yl]-2,8-dimethyl-1,10-dioxaspiro[4.5]decan-9-yl]-2-methyl-3-propanoyloxypentanoic acid Chemical compound C1C(O)C(C)C(C(C)C(OC(=O)CC)C(C)C(O)=O)OC11OC(C)(C2OC(C)(CC2)C2C(CC(O2)C2C(CC(C)C(O)(CO)O2)C)C)CC1 ZNBNBTIDJSKEAM-UHFFFAOYSA-N 0.000 claims description 3
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 3
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- VEFXTGTZJOWDOF-UHFFFAOYSA-N benzene;hydrate Chemical compound O.C1=CC=CC=C1 VEFXTGTZJOWDOF-UHFFFAOYSA-N 0.000 claims description 3
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004327 boric acid Substances 0.000 claims description 3
- YPTUAQWMBNZZRN-UHFFFAOYSA-N dimethylaminoboron Chemical compound [B]N(C)C YPTUAQWMBNZZRN-UHFFFAOYSA-N 0.000 claims description 3
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 3
- POCUPXSSKQAQRY-UHFFFAOYSA-N hydroxylamine;hydrate Chemical compound O.ON POCUPXSSKQAQRY-UHFFFAOYSA-N 0.000 claims description 3
- 229910000378 hydroxylammonium sulfate Inorganic materials 0.000 claims description 3
- VHNQIURBCCNWDN-UHFFFAOYSA-N pyridine-2,6-diamine Chemical compound NC1=CC=CC(N)=N1 VHNQIURBCCNWDN-UHFFFAOYSA-N 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 11
- 238000000576 coating method Methods 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 7
- 239000000853 adhesive Substances 0.000 abstract description 6
- 230000001070 adhesive effect Effects 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 20
- 238000012360 testing method Methods 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 14
- 238000012545 processing Methods 0.000 description 8
- 239000000758 substrate Substances 0.000 description 6
- 239000003973 paint Substances 0.000 description 4
- 238000009210 therapy by ultrasound Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 description 2
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 2
- 229910021538 borax Inorganic materials 0.000 description 2
- 229910000365 copper sulfate Inorganic materials 0.000 description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- LBVZYUZDHIPGLN-UHFFFAOYSA-N imidazol-1-ylmethanethiol Chemical compound SCN1C=CN=C1 LBVZYUZDHIPGLN-UHFFFAOYSA-N 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000001465 metallisation Methods 0.000 description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 2
- -1 palladium ions Chemical class 0.000 description 2
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 description 2
- 239000001509 sodium citrate Substances 0.000 description 2
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 description 2
- 235000011006 sodium potassium tartrate Nutrition 0.000 description 2
- 239000004328 sodium tetraborate Substances 0.000 description 2
- 235000010339 sodium tetraborate Nutrition 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229940074439 potassium sodium tartrate Drugs 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 235000011083 sodium citrates Nutrition 0.000 description 1
- 239000001476 sodium potassium tartrate Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 210000003813 thumb Anatomy 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1851—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material
- C23C18/1872—Pretreatment of the material to be coated of surfaces of non-metallic or semiconducting in organic material by chemical pretreatment
- C23C18/1886—Multistep pretreatment
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/38—Coating with copper
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
The invention provides a method for chemically plating copper on the surface of glass. The method for chemically plating copper on the surface of the glass comprises the following steps: (1) carrying out ultrasonic cleaning on the glass, and then adjusting; (2) performing pre-dipping treatment on the glass treated in the step (1); (3) activating and reducing the glass treated in the step (2); (4) placing the glass treated in the step (3) in a chemical nickel plating solution for chemical nickel plating, and then drying; (5) and (4) immersing the glass treated in the step (4) into a chemical copper plating solution for chemical copper plating, and drying to obtain a finished product. The method provided by the invention simplifies the process flow, reduces the cost and reduces the environmental pollution; and the treated glass material metal layer has good uniformity and high adhesive force, and can effectively avoid the separation of the coating and the glass.
Description
Technical Field
The invention belongs to the field of printed circuit board processing, and particularly relates to a method for chemically plating copper on the surface of glass.
Background
With the development of IC carriers, the selection of the material of the interposer and the metallization thereof are one of the problems to be solved. In recent years, many studies have indicated that glass is a potential interposer material with the advantages of low dielectric constant and easy access to large area substrates. Although glass seems to be the most excellent interposer material, the current technology of using glass as an interposer material for fabricating conductive lines is late and cannot be mass-produced, one of which is difficult due to the poor adhesion of the metallization process. Traditionally, adhesion of the metal coating is usually provided by roughness of the substrate surface, but the surface roughness of the glass is very low, so the adhesion of the coating becomes one of the keys for successful introduction of the interlayer material into the glass.
CN106242314A discloses a glass copper plating process, which comprises the following steps: and spraying conductive paint on the area of the glass surface needing copper plating to form a conductive layer, and then plating copper on the surface of the conductive layer. According to the glass copper plating process, before the conductive paint is sprayed, the surface of the glass is not subjected to any chemical treatment, the surface of the glass is cleaned by tap water, and when the conductive paint is sprayed on the surface of the glass, copper plating is performed after the conductive paint is dried, so that the sprayed surface is uniform and smooth, and the uniformity of copper plating on the surface of the glass is ensured, so that the whole coating film is continuously and uniformly plated with good conductivity. Although the process is simple, the adhesion of the plating layer is poor.
CN107225329A discloses a method for improving copper plating connection strength of glass, which adopts excimer laser processing to roughen the surface of a glass substrate and can obviously improve the connection strength between a plating layer and the glass substrate. The laser processing effect is controlled by changing the parameter setting during laser processing, different microstructure arrays are generated on the surface, then the surface appearance of the glass after treatment is measured by adopting three-dimensional surface appearance and three-dimensional parameter representation, the adhesion strength of copper plating is evaluated by a scratch test, the laser processing energy is favorably used to the maximum, the processing time is saved, the processing effect is controlled, an ideal roughened surface is achieved, and the quality of glass coating is obviously improved. According to the method, after the surface of the glass substrate is roughened by excimer laser processing, the connection strength between the coating and the glass substrate can be remarkably improved, but the method is complicated in steps, complex in operation and high in cost.
Therefore, it is highly desirable to develop a method that can improve the adhesion of the coating and has a simple process and easy operation to meet the application requirements.
Disclosure of Invention
Aiming at the problems of poor binding force between a plating layer and glass, separation of the plating layer and the like in the prior art, the invention aims to provide a method for chemically plating copper on the surface of the glass.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for electroless copper plating on a glass surface, comprising the following steps:
(1) carrying out ultrasonic cleaning on the glass, and then adjusting;
(2) performing pre-dipping treatment on the glass treated in the step (1);
(3) activating and reducing the glass treated in the step (2);
(4) placing the glass treated in the step (3) in a chemical nickel plating solution for chemical nickel plating, and then drying;
(5) and (4) immersing the glass treated in the step (4) into a chemical copper plating solution for chemical copper plating, and drying to obtain a finished product.
The method can effectively avoid the problem of poor binding force between the electroplated copper and nickel and the glass through the steps of adjustment, activation and reduction, ensures that the coating is uniform and is well combined with the glass, can protect the copper and nickel layer from being corroded, is favorable for the deposition of the copper and nickel, and avoids the phenomenon of plating leakage.
Preferably, the step of ultrasonic cleaning in step (1) comprises the step of putting the glass in absolute ethyl alcohol for ultrasonic soaking treatment.
Preferably, the ultrasonic frequency is 35-45kHz, for example, 36kHz, 37kHz, 38kHz or 39kHz, and specific values within the above numerical ranges can be selected, which are not described herein again.
Preferably, the soaking temperature is 20-30 ℃ (for example, may be 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 27 ℃, 28 ℃ or 29 ℃) and the time is 2-5min (for example, may be 2min, 2.5min, 3min, 3.5min, 4min or 4.5 min), and specific values within the above numerical ranges may be selected, which is not described herein again.
Preferably, the adjustment comprises a first adjustment and a second adjustment.
The method of the invention is adjusted and processed for two times, so that the fine operation can ensure that no impurities are left on the surface of the glass on one hand, and a layer of organic matter can be adsorbed on the surface of the glass on the other hand, thereby adjusting the charge on the surface of the glass, being beneficial to the subsequent activation treatment and further ensuring the uniformity of the subsequent copper plating on the surface of the glass.
Preferably, the first conditioning step comprises the step of soaking the glass subjected to ultrasonic cleaning in a conditioning solution 1, wherein the conditioning solution 1 comprises hydroxylamine sulfate and water.
Preferably, the soaking temperature is 40-50 ℃ (for example, 41 ℃, 42 ℃, 43 ℃, 44 ℃, 45 ℃, 46 ℃, 47 ℃, 48 ℃ or 49 ℃) and the time is 1-3min (for example, 1.2min, 1.5min, 1.8min, 2min, 2.5min or 2.8 min), and specific values in the above numerical ranges can be selected, which is not described again.
Preferably, the step of adjusting for the second time comprises the step of putting the glass subjected to the first adjusting treatment into an adjusting liquid 2 for soaking treatment, wherein the adjusting liquid 2 comprises the components of ethylenediamine, sodium hydroxide and water.
Preferably, the soaking temperature is 50-55 ℃ (for example, 51 ℃, 52 ℃, 53 ℃, 54 ℃, or 55 ℃) and the soaking time is 1-3min (for example, 1.2min, 1.5min, 1.8min, 2min, 2.5min, or 2.8 min), and specific values in the above numerical ranges can be selected, and are not described again.
Preferably, the step of pre-dipping of step (2) comprises: and (3) putting the glass subjected to the second adjustment treatment into a pre-soaking solution for soaking treatment, wherein the pre-soaking solution comprises the components of sodium dodecyl sulfate and water.
Preferably, the soaking temperature is 20-30 ℃ (for example, may be 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 27 ℃, 28 ℃ or 29 ℃) and the soaking time is 20-60s (for example, may be 25s, 30s, 35s, 40s, 45s, 50s or 55 s), and specific values in the above numerical ranges may be selected, which is not described herein again.
The method of the invention can improve the wettability of the glass surface by performing the pre-dipping treatment before the activation treatment of the glass, and can better improve the adsorption of palladium ions during the activation.
Preferably, the step of activating treatment of step (3) comprises: and (3) putting the glass subjected to the pre-soaking treatment into an activating solution for activating treatment, wherein the activating solution comprises a complexing agent, palladium sulfate, sodium dodecyl benzene sulfonate and water.
Preferably, the complexing agent comprises any one or a combination of at least two of 2, 6-diaminopyridine, disodium ethylenediaminetetraacetate or triethanolamine.
Preferably, the pH of the activation solution is 8.5 to 9.5.
Preferably, the temperature of the activation treatment is 45-55 ℃ (for example, 45 ℃, 46 ℃, 47 ℃, 48 ℃, 49 ℃, 50 ℃, 52 ℃ or 54 ℃ and the like), the time is 1-3min (for example, 1.2min, 1.5min, 1.8min, 2min, 2.5min or 2.8min and the like), and specific values in the above numerical value ranges can be selected, which is not described again.
Preferably, the step of reduction treatment in step (3) comprises: and (3) putting the activated glass into a reducing solution for reduction treatment, wherein the reducing solution comprises dimethylamino borane, boric acid and water.
Preferably, the temperature of the reduction treatment is 30-40 ℃ (for example, 31 ℃, 32 ℃, 33 ℃, 34 ℃, 35 ℃, 36 ℃, 37 ℃, 38 ℃ or 39 ℃) and the time is 1-2min (for example, 1.1min, 1.2min, 1.4min, 1.5min, 1.7min or 1.9 min), and specific values in the above numerical ranges can be selected, and thus, the detailed description is omitted here.
Preferably, the chemical nickel plating solution in step (4) comprises nickel sulfate, sodium hypophosphite, sodium citrate, sodium tetraborate, lactic acid and water, and specific values within the above numerical ranges can be selected, and are not repeated herein.
Preferably, the stabilizer comprises thiomethyl imidazole and/or 2, 2-bipyridine.
Preferably, the pH of the electroless nickel plating solution is 4.5-5.5.
Preferably, the electroless nickel plating temperature is 60-70 ℃ (for example, 61 ℃, 62 ℃, 63 ℃, 64 ℃, 65 ℃, 66 ℃, 67 ℃, 68 ℃ or 69 ℃) and the time is 1-3min (for example, 1.2min, 1.5min, 1.8min, 2min, 2.5min or 2.8 min), and specific values in the above numerical value ranges can be selected, and are not described again.
Preferably, the step of cleaning the glass after the chemical nickel plating by using deionized water is further included after the chemical nickel plating.
Preferably, the drying of step (4) includes: and (3) baking the glass subjected to the chemical nickel plating treatment in an oven.
Preferably, the baking temperature is 110-.
Preferably, the components of the electroless copper plating solution in the step (5) include sodium potassium tartrate, copper sulfate, formaldehyde, a stabilizer and water, and specific values within the above numerical value ranges can be selected, which are not described in detail herein.
Preferably, the stabilizer comprises thiomethyl imidazole and/or 2, 2-bipyridine.
Preferably, the pH of the electroless copper plating solution is 11.5 to 13.
Preferably, the electroless copper plating temperature is 30-35 ℃ (for example, may be 31 ℃, 32 ℃, 33 ℃, 34 ℃ or 35 ℃) and the time is 4-8min (for example, may be 4.5min, 5min, 5.5min, 6min, 6.5min, 7min or 7.5 min), and specific values in the above numerical ranges may be selected, which is not described herein again.
Preferably, the step of cleaning the glass after the electroless copper plating by using deionized water is further included after the electroless copper plating.
Preferably, the drying of step (5) includes: and (3) baking the glass subjected to the chemical copper plating treatment in an oven.
Preferably, the baking temperature is 100-.
Preferably, the method for electroless copper plating on the surface of the glass comprises the following steps:
(1) ultrasonic treatment: putting the glass into absolute ethyl alcohol for ultrasonic soaking treatment, and then putting the glass into deionized water for cleaning; the ultrasonic frequency is 35-45kHz, the soaking temperature is 20-30 ℃, and the soaking time is 2-5 min;
(2) and (3) adjusting: soaking the glass treated in the step (1) in the conditioning solution 1 at 40-50 ℃ for 1-3min for carrying out first conditioning treatment; cleaning with deionized water, soaking in the adjusting solution 2 at 50-55 deg.C for 1-3min for second adjusting treatment;
(3) pre-dipping: cleaning the glass treated in the step (2) by using deionized water, and then soaking the glass in a presoaking solution for 20-60s at the temperature of 20-30 ℃;
(4) activation reduction treatment: cleaning the glass treated in the step (3) with deionized water, putting the glass into an activating solution, activating for 1-3min at 45-55 ℃, cleaning with deionized water, putting the glass into a reducing solution, and reducing for 1-2min at 30-40 ℃;
(5) chemical nickel plating: cleaning the glass treated in the step (4) by using deionized water, placing the glass in a chemical nickel plating solution for chemical nickel plating for 1-3min at 60-70 ℃, cleaning by using deionized water, placing the glass in an oven for baking for 5-10min at 110-130 ℃, and then cleaning by using deionized water;
(6) chemical copper plating: immersing the glass treated in the step (5) into chemical copper plating solution, chemically plating copper for 4-8min at 30-34 ℃, cleaning with deionized water, placing in an oven, baking for 5-10min at 100-120 ℃, and cleaning with deionized water to obtain the finished product.
Compared with the prior art, the invention has the following beneficial effects:
the method for chemically plating copper on the surface of the glass provided by the invention can effectively avoid the problem of poor bonding force between electroplated copper and nickel and the glass by adopting the steps of adjustment, activation and reduction, ensures that a plating layer is uniform and is well bonded with the glass, can protect the copper and nickel layer from being corroded, is beneficial to the deposition of the copper and nickel, avoids the phenomenon of plating leakage, ensures that the uniformity of a metal layer of a glass material obtained by treatment is good, simplifies the process flow, reduces the cost and reduces the environmental pollution.
Drawings
Fig. 1 is a picture after the tape adhesion test of example 1.
Fig. 2 is a picture after the tape adhesion test of example 2.
Fig. 3 is a picture after the tape adhesion test of example 3.
Fig. 4 is a picture after the tape adhesion test of example 4.
Fig. 5 is a picture after the tape adhesion test of example 5.
Fig. 6 is a picture after the tape adhesion test of example 6.
Fig. 7 is a picture after the tape adhesion test of example 7.
Fig. 8 is a picture after the tape adhesion test of comparative example 1.
Fig. 9 is a picture after the tape adhesion test of comparative example 2.
Fig. 10 is a picture after the tape adhesion test of comparative example 3.
Fig. 11 is a picture after the tape adhesion test of comparative example 4.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Some of the reagents used in the following examples were sourced as follows:
the conditioning solution 1 was: SkySecure 312C solution (the components are 10g/L of hydroxylamine sulfate and water) prepared by Shanghai skywrit chemical company;
the adjusting liquid 2 is SkyClean 321C (the components are 20g/L of ethylenediamine, 15g/L of sodium hydroxide and water) prepared by Shanghai sky-borne chemical company Limited;
the pre-soaking solution is SkyCat330C solution (the components are 0.05g/L of sodium dodecyl sulfate and water) prepared by Shanghai Tian Cheng chemical company Limited;
the activating solution is SkyCat335C (the components are 0.06g/L of 2, 6-diaminopyridine, 0.06g/L of disodium ethylene diamine tetraacetate, 0.06g/L of triethanolamine, 0.2g/L of palladium sulfate, 0.03g/L of sodium dodecyl benzene sulfonate and water) prepared by Shanghai Tian-Zhi chemical company Limited;
the reducing solution is SkyCat 336R solution (the components are 15g/L of dimethylamino borane, 10g/L of boric acid and water) prepared by Shanghai Tian Cheng chemical company Limited;
the chemical nickel plating solution is SkyPosit Ni920 solution (comprising 50g/L nickel sulfate, 20g/L sodium hypophosphite, 15g/L sodium citrate, 25g/L sodium tetraborate, 15g/L lactic acid and water) prepared by Shanghai Tiansui chemical Limited company, and the pH value is 5.0;
the chemical copper plating solution is SkyCopp 3652 solution (the components are potassium sodium tartrate 60g/L, copper sulfate 10g/L, formaldehyde 20g/L, sulfenyl methyl imidazole 0.05g/L and water) prepared by Shanghai sky-borne chemical company Limited, and the pH value is 12.
Example 1
The embodiment provides a method for electroless copper plating on the surface of glass, which comprises the following steps:
(1) ultrasonic treatment: putting the glass into absolute ethyl alcohol for ultrasonic soaking treatment, and then putting the glass into deionized water for cleaning; the ultrasonic frequency is 40KHz, the soaking temperature is 25 ℃, and the time is 3 min;
(2) and (3) adjusting: soaking the glass treated in the step (1) in a SkySecure 312C solution at 45 ℃ for 2min for carrying out first adjustment treatment; cleaning with deionized water, soaking in SkyClean 321C solution at 55 deg.C for 2min for second adjustment treatment;
(3) pre-dipping: washing the glass treated in the step (2) with deionized water, and soaking the glass in SkyCat330C solution at 25 ℃ for 40S;
(4) activation reduction treatment: cleaning the glass treated in the step (3) with deionized water, then putting the glass into a SkyCat335C solution, activating the glass for 2min at 50 ℃, cleaning the glass with deionized water, then putting the glass into a SkyCat 336R solution, and reducing the glass for 1-2min at 35 ℃;
(5) chemical nickel plating: cleaning the glass treated in the step (4) with deionized water, placing the glass in SkyPosit Ni920 solution, performing chemical nickel plating for 2min at 65 ℃, cleaning with deionized water, placing the glass in an oven, baking for 8min at 120 ℃, and then cleaning with deionized water;
(6) chemical copper plating: and (3) immersing the glass treated in the step (5) into a SkyCopp 3652 solution, chemically plating copper for 5min at 32 ℃, cleaning with deionized water, baking in an oven at 110 ℃ for 8min, and cleaning with deionized water to obtain a finished product.
Example 2
The embodiment provides a method for electroless copper plating on the surface of glass, which comprises the following steps:
(1) ultrasonic treatment: putting the glass into absolute ethyl alcohol for ultrasonic soaking treatment, and then putting the glass into deionized water for cleaning; the ultrasonic frequency is 45KHz, the soaking temperature is 30 ℃, and the time is 2 min;
(2) and (3) adjusting: soaking the glass treated in the step (1) in a SkySecure 312C solution at 40 ℃ for 3min for first adjustment treatment; cleaning with deionized water, soaking in SkyClean 321C solution at 52 deg.C for 1min for second adjustment treatment;
(3) pre-dipping: washing the glass treated in the step (2) with deionized water, and then soaking the glass in SkyCat330C solution at 30 ℃ for 60S;
(4) activation reduction treatment: cleaning the glass treated in the step (3) with deionized water, putting the glass into a SkyCat335C solution, activating the glass for 1min at 55 ℃, cleaning the glass with deionized water, putting the glass into a SkyCat 336R solution, and reducing the glass for 2min at 30 ℃;
(5) chemical nickel plating: cleaning the glass treated in the step (4) by using deionized water, placing the glass into SkyPosit Ni920 solution, carrying out chemical nickel plating for 1min at 70 ℃, cleaning the glass by using deionized water, placing the glass into an oven, baking the glass for 10min at 110 ℃, and then cleaning the glass by using deionized water;
(6) chemical copper plating: and (3) immersing the glass treated in the step (5) into a SkyCopp 3652 solution, chemically plating copper for 8min at 30 ℃, cleaning with deionized water, baking in an oven at 120 ℃ for 5min, and cleaning with deionized water to obtain a finished product.
Example 3
The embodiment provides a method for electroless copper plating on the surface of glass, which comprises the following steps:
(1) ultrasonic treatment: putting the glass into absolute ethyl alcohol for ultrasonic soaking treatment, and then putting the glass into deionized water for cleaning; the ultrasonic frequency is 35KHz, the soaking temperature is 20 ℃, and the time is 5 min;
(2) adjusting: soaking the glass treated in the step (1) in a SkySecure 312C solution at 50 ℃ for 1min for first adjustment treatment; cleaning with deionized water, soaking in SkyClean 321C solution at 50 deg.C for 3min for second adjustment treatment;
(3) pre-dipping: washing the glass treated in the step (2) with deionized water, and soaking the glass in SkyCat330C solution at 20 ℃ for 20S;
(4) activation reduction treatment: cleaning the glass treated in the step (3) with deionized water, putting the glass into a SkyCat335C solution, activating the glass for 3min at 45 ℃, cleaning the glass with deionized water, putting the glass into a SkyCat 336R solution, and reducing the glass for 1min at 40 ℃;
(5) chemical nickel plating: cleaning the glass treated in the step (4) with deionized water, placing the glass in SkyPosit Ni920 solution, performing chemical nickel plating for 3min at the temperature of 60 ℃, cleaning with deionized water, placing the glass in an oven, baking for 5min at the temperature of 130 ℃, and then cleaning with deionized water;
(6) chemical copper plating: and (4) immersing the glass treated in the step (5) into a SkyCopp 3652 solution, chemically plating copper for 4min at 34 ℃, cleaning with deionized water, baking for 10min in an oven at 100 ℃, and cleaning with deionized water to obtain a finished product.
Example 4
This example provides a method for electroless copper plating on a glass surface, which differs from example 1 only in that only the first conditioning treatment is performed in step (2) and the conditioning time is kept for 4min, and the remaining steps are identical to example 1.
Example 5
This example provides a method for electroless copper plating of a glass surface which differs from example 1 only in that only the second conditioning treatment is carried out in step (2) and the conditioning time is kept for 4min, the remaining steps being identical to example 1.
Example 6
This example provides a method for electroless copper plating on a glass surface, which differs from example 1 only in that the conditioning solution in the second conditioning treatment in step (2) is a SkySecure 312C solution, and the remaining steps are identical to example 1.
Example 7
This example provides a method for electroless copper plating on a glass surface, which differs from example 1 only in that the conditioning solution at the first conditioning treatment in step (2) is a SkyClean 321C solution, and the remaining steps are identical to example 1.
Comparative example 1
This comparative example provides a method for electroless copper plating on a glass surface which differs from example 1 only in that the conditioning treatment of step (2) is not included, and the remaining steps are in agreement with example 1.
Comparative example 2
This comparative example provides a method for electroless copper plating on glass surfaces which differs from example 1 only in the prepreg which does not include step (3), the remaining steps remaining in accordance with example 1.
Comparative example 3
This comparative example provides a method for electroless copper plating on a glass surface, which differs from example 1 only in that the activation-reduction treatment of step (4) is not included, and the remaining steps are kept in agreement with example 1.
Comparative example 4
This comparative example provides a method for electroless copper plating on a glass surface, which differs from example 1 only in that the reduction treatment of step (4) is not included, and the remaining steps are kept in agreement with example 1.
Test example
The copper-coated glasses obtained by the methods of examples 1 to 7 and comparative examples 1 to 4 were tested by the following methods:
testing adhesive force of the adhesive tape:
(1) pasting an adhesive tape on the chemical copper plating layer on the surface of the glass;
(2) peeling the tape at an angle of 180 ° with firm pressure applied with the thumb;
(3) repeating the steps (1) and (2) for 6 times, and judging the adhesive force of the chemical plating layer according to the final stripping grade.
Note: grade 1 is that the adhesive force of the coating is strong, and 0-10% of the test area is peeled off;
grade 2 is that the coating has good adhesive force, and 10-30% of the test area is stripped;
grade 3 is that the adhesive force of the plating layer is general, and 30-70% of the test area is stripped;
grade 4 is that the adhesion of the coating is very poor, and 70-100% of the test area is stripped.
The results are shown in the following table:
from the data in the table and the attached figures, it can be seen that: the copper-plated glass obtained by the method of examples 1 to 3 had a copper-plated layer peeling area within 10%, which indicates that the glass surface plated with copper by the method of the present invention had a strong bonding force with the plating layer
The copper-plated glass obtained by the method of examples 4-7 has a copper-plated layer peeling area of 10% -30%, which indicates that the use of the conditioning solution in the conditioning treatment in the method of the present application affects the bonding force between the glass and the plating layer;
the area of the copper-plated glass copper-plated layer obtained by the method of comparative examples 1-4 is more than 70%, which shows that the method of the application has the defects that the steps are connected in a ring-to-ring manner, and the bonding force between the glass and the plating layer is reduced without performing adjustment treatment, pre-dipping treatment and activation reduction treatment.
The applicant states that the present invention is illustrated by the above examples of a method of electroless copper plating on a glass surface according to the present invention, but the present invention is not limited to the above examples, i.e., it is not meant to imply that the present invention must be practiced by relying on the above examples. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
Claims (10)
1. The method for chemically plating copper on the surface of glass is characterized by comprising the following steps of:
(1) carrying out ultrasonic cleaning on the glass, and then adjusting;
(2) performing pre-dipping treatment on the glass treated in the step (1);
(3) activating and reducing the glass treated in the step (2);
(4) placing the glass treated in the step (3) in a chemical nickel plating solution for chemical nickel plating, and then drying;
(5) and (4) immersing the glass treated in the step (4) into a chemical copper plating solution for chemical copper plating, and drying to obtain a finished product.
2. The method for electroless copper plating on the surface of glass according to claim 1, wherein the step of ultrasonic cleaning in step (1) comprises the steps of placing the glass in absolute ethyl alcohol for ultrasonic soaking treatment;
preferably, the ultrasonic frequency is 35-45kHz, the soaking temperature is 20-30 ℃, and the soaking time is 2-5 min.
3. The method of electroless copper plating on glass surfaces according to claim 1 or 2, wherein the conditioning comprises a first conditioning and a second conditioning;
preferably, the step of first adjustment comprises the step of soaking the glass subjected to ultrasonic cleaning in an adjustment liquid 1, wherein the adjustment liquid 1 comprises hydroxylamine sulfate and water;
preferably, the soaking temperature is 40-50 ℃, and the soaking time is 1-3 min;
preferably, the step of adjusting for the second time comprises the step of putting the glass subjected to the first adjusting treatment into an adjusting liquid 2 for soaking treatment, wherein the adjusting liquid 2 comprises the components of ethylenediamine, sodium hydroxide and water;
preferably, the soaking temperature is 50-55 ℃ and the soaking time is 1-3 min.
4. A method for electroless copper plating of glass surfaces according to any of claims 1-3 wherein the step of pre-dipping in step (2) comprises: putting the glass subjected to the second adjustment treatment into a pre-soaking solution for soaking treatment, wherein the pre-soaking solution comprises the components of sodium dodecyl sulfate and water;
preferably, the soaking temperature is 20-30 ℃ and the soaking time is 20-60 s.
5. The method for electroless copper plating on glass surfaces according to any of the claims 1 to 4, wherein the step of activating treatment of step (3) comprises: putting the presoaked glass into an activating solution for activating treatment, wherein the activating solution comprises a complexing agent, palladium sulfate, sodium dodecyl benzene sulfonate and water;
preferably, the complexing agent comprises any one or a combination of at least two of 2, 6-diaminopyridine, disodium ethylenediaminetetraacetate or triethanolamine;
preferably, the pH of the activation solution is 8.5-9.5;
preferably, the temperature of the activation treatment is 45-55 ℃ and the time is 1-3 min.
6. The method for electroless copper plating on glass surfaces according to any of the claims 1 to 5, wherein the step of reduction treatment of step (3) comprises: putting the activated glass into a reducing solution for reduction treatment, wherein the reducing solution comprises dimethylamino borane, boric acid and water;
preferably, the temperature of the reduction treatment is 30-40 ℃ and the time is 1-2 min.
7. The method for electroless copper plating on glass surfaces according to any of the claims 1-6, wherein the temperature of the electroless nickel plating in the step (4) is 60-70 ℃ and the time is 1-3 min;
preferably, the step of cleaning the glass after the chemical nickel plating by using deionized water is further included after the chemical nickel plating.
8. The method for electroless copper plating on glass surfaces according to any of the claims 1 to 7, wherein the drying of step (4) comprises: placing the glass subjected to the chemical nickel plating treatment in an oven for baking;
preferably, the baking temperature is 110-.
9. The method for electroless copper plating on glass surface according to any of the claims 1-8, wherein the temperature of the electroless copper plating in the step (5) is 30-34 ℃ and the time is 4-8 min;
preferably, the step of cleaning the glass after the electroless copper plating by using deionized water is further included after the electroless copper plating.
10. The method for electroless copper plating on glass surfaces according to any of the claims 1 to 9, wherein the drying of step (5) comprises: placing the glass subjected to the chemical copper plating treatment in an oven for baking;
preferably, the baking temperature is 100-120 ℃, and the baking time is 5-10 min.
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