CN110195222A - A kind of RTR subtracts copper post-processing copper foil surface passivator and its use and preparation method - Google Patents
A kind of RTR subtracts copper post-processing copper foil surface passivator and its use and preparation method Download PDFInfo
- Publication number
- CN110195222A CN110195222A CN201910479282.0A CN201910479282A CN110195222A CN 110195222 A CN110195222 A CN 110195222A CN 201910479282 A CN201910479282 A CN 201910479282A CN 110195222 A CN110195222 A CN 110195222A
- Authority
- CN
- China
- Prior art keywords
- copper foil
- rtr
- passivator
- foil surface
- subtracts
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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
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/68—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous solutions with pH between 6 and 8
-
- 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
Abstract
A kind of RTR subtracts copper post-processing copper foil surface passivator and its use and preparation method, the present invention relates to a kind of RTR to subtract copper post-processing copper foil surface passivator, subtract the defect of improvement poor corrosion resistance after copper for improvement, the present invention uses following technology: a kind of RTR subtracts copper post-processing copper foil surface passivator composition, it includes the component of following mass parts: antioxidant 15-20g/L, complexing agent 3-5g/L, surfactant 0.1-0.3g/L, solvent 30-45g/L, dispersing agent 0.1-0.3g/L, rare earth metal source 0.5-1.0g/L, adhere to reinforcing agent 0.8-1.2g/L, pH buffer (holding pH value is 6.5-7.5), reducing agent 0.05-0.1g/L, water.The beneficial effects of the present invention are: more main effect is embodied in the antioxygenic property using passivating technique extension copper foil base material, so that flexible circuit board copper foil in board making process subtract copper process section after, it can be kept in depending on the condition of production, without working continuously on site because the reason of before subtracting copper process section limits.
Description
Technical field
The present invention relates to a kind of RTR to subtract copper post-processing copper foil surface passivator, relates in particular to wiring board FPC and subtracts copper
Process section copper foil surface anti-corrosion treatment technology.
Background technique
Printed circuit board, also known as printed circuit board are the suppliers of electronic component electrical connection.Its development is existing
More than 100 years history；Major advantage using circuit board is to greatly reduce the mistake of wiring and assembly, improves Automated water
Gentle productive labor rate.To the development of the national economy, national defense construction and social development with vital strategic position and not
Alternative effect.Printed circuit board is to be made with copper clad laminate (Copper-clad Laminate abbreviation CCL) as raw material
The important mechanism component of the electric appliance or electronics made.Specifically, substrate is by dielectric layer (resin Resin, glass fibre Glass
), and the composite material (Composite that is constituted of both conductors of high-purity (copper foil Copper foil) fiber
material).The quality of copper foil affects subsequent terminal product quality, therefore the process of surface treatment for carrying out copper foil is critically important.
The basic procedure handled at present: oil removing (polish-brush)-washing-copper-washing-drying is thinned, copper foil is subtracting copper process section
Afterwards, surface becomes coarse because being etched, and the aerial area of copper foil surface exposure is bigger, aerial oxidation corrosion speed
Degree is accelerated, and leads to copper foil surface nigrescence floating, influences the final quality of product, therefore by adding passivation after subtracting copper process section
Slot realizes the online passivation technology of CCL, is passivated process to copper material surface to reach corrosion-resisting function.For a long time,
Most of passivating solutions used are all chromic acid or BTA (benzotriazole).Personal safety in operating process, to staff
With certain threat；Also, the chromium acid waste liquid processing difficulty after being passivated is larger, and environmental pollution is larger after discharge, and BTA
The passivating solution of system have certain corrosion resistance, but its passivation formed passivating film film forming speed it is slow, need to impregnate when
Between it is relatively long, be not suitable for the automatic limp technique of online RTR, also, the film acid resistance ability after forming a film is poor, finding one kind can
There is fast filming the passivating solution of good corrosion resistance to subtract copper process with good realistic meaning to RTR again.
Summary of the invention
The object of the invention is to the deficiencies in order to solve the prior art, and providing can efficiently inhibit copper foil surface rotten
The passivator solution formula of erosion, a kind of RTR for improving the defect of poor corrosion resistance subtract copper post-processing copper foil surface passivator.
The present invention is attained in that using following technical solution
A kind of RTR subtracts copper post-processing copper foil surface passivator composition, it includes the component of following mass parts: anti-oxidant
It is agent 15-20g/L, complexing agent 3-5g/L, surfactant 0.1-0.3g/L, solvent 30-45g/L, dispersing agent 0.1-0.3g/L, dilute
Earth metal source 0.5-1.0g/L, attachment reinforcing agent 0.8-1.2g/L, pH buffer (holding pH value is 6.5-7.5), reducing agent
0.05-0.1g/L, water.
Specifically, in which:
The antioxidant is benzotriazole, 15-20g/L；
The complexing agent is edetate disodium, tetrasodium ethylenediamine tetraacetate, ethylenediamine, monoethanolamine, diethanol
Amine, triethanolamine, ammonium sulfate, ammonium chloride, citrate, pyrophosphate, tartrate, sulphite, thiosulfate, grape
One of sodium saccharate etc. is a variety of, preferably one of disodium ethylene diamine tetraacetate, triethanolamine, tartrate or a variety of,
3-5g/L；
The surfactant is in fatty alcohol polyoxyethylene ether, aliphatic amine polyoxyethylene ether and castor oil phosphate ester
It is one or more, 0.1-0.3g/L；
The solvent is the mixing of one of dehydrated alcohol, isopropyl acetate and isomery lauryl alcohol or two kinds or more,
30-45g/L；
The dispersing agent is one of sodium tripolyphosphate, polyacrylamide, methyl anyl alcohol or a variety of, 0.1-0.3g/
L；
The rare earth metal source is one of lanthanum nitrate, nitric acid cerium salt, 0.5-1.0g/L；
Described adheres to reinforcing agent for the mixing with sulfuric acid solution one or two kinds of in monoethanolamine, butyl
Object, 0.8-1.2g/L；
The pH buffer be hydroxide, sulfuric acid, citric acid, hydrochloric acid, boric acid, acetic acid, ammonium hydroxide, disodium hydrogen phosphate,
One or more, preferably hydroxide, sulfuric acid, the lemon of dipotassium hydrogen phosphate, sodium dihydrogen phosphate, potassium dihydrogen phosphate, acetate etc.
One of acid, sodium dihydrogen phosphate, potassium dihydrogen phosphate, acetate are a variety of, 6.5-7.5.
The reducing agent is one of sulphite, sodium hypophosphite, boron hydride, hydrazine hydrate etc. or a variety of, excellent
Select one or more, the 0.05-0.1g/L of sulphite, sodium hypophosphite.
Remaining is pure water.
Specific steps:
A. the antioxidant of proportion mass parts is added into the solvent solution of proportion mass concentration, 15-20g/L is sufficiently stirred
Mix it is uniformly mixed, can suitably heat (water-bath, temperature≤50 DEG C) help dissolve；
B. the rare earth metal source salt of proportion mass parts, 0.5-1.0g/L are added into above-mentioned mixed solution；
C. the complexing agent of proportion mass parts is added into above-mentioned mixed solution, mass fraction 3-5g/L is mixed evenly；
D. the activator of proportion mass parts is added into above-mentioned mixed solution, 0.1-0.3g/L is mixed evenly；
E. the dispersing agent of proportion mass parts is added into above-mentioned mixed solution, 0.1-0.3g/L is mixed evenly；
F. the attachment reinforcing agent of proportion mass parts is added into above-mentioned mixed solution, 0.8-1.2/L is mixed evenly；
G. the pH buffer solvent of proportion mass parts is added, so that solution pH value is between 6.5-7.5；
H. surplus is pure water, constant volume.
The application method of passivator in the present invention: a kind of RTR subtracts copper post-processing copper foil surface passivator in use process
In using passivator contact substrate surface be principle progress produced on-site operation.
When specific operation,
1) the optional level of plate mode is put to put plate or vertically put plate；
2) the spray perhaps immersion wherein optional single face spraying of spray or two-sided spray may be selected in the way of contact；
3) passivator time of contact: the time of contact of spray is 5-10 minutes, and the time of immersion is 3-5 minutes；
4) passivator operating temperature: 30 ± 10 DEG C；
5) fountain, operating pressure: 0.8-1.2 (kg/cm2)；Using immersion type, passivator is needed not have substrate completely；
6) continue to be sent to next process section by transmitting by the copper foil that deactivation slot completes passivation.
Complete process flow diagram after adding passivation is as follows:
Feeder → DI water → oil removing → pressure washing 1,2,3 → subtracts copper → pressure washing 4,5,6 → passivation → pressure water
It washes 7,8,9 → blots → high wind drying → hot blast drying → cooling → collecting machine.
The beneficial effects of the present invention are: more main effect is embodied in the antioxygen using passivating technique extension copper foil base material
Change performance so that flexible circuit board copper foil in board making process subtract copper process section after, can be carried out depending on the condition of production temporary
It deposits, without (stinging copper, surface is subtracted the immersion of copper agent liquid medicine at this time, fine and closely woven cavity is left, in sky because before subtracting copper process section
Inoxidizability in gas is very low, and natural storage time can be observed visually apparent discoloration in one day, that is, it is sub- to be oxidized to oxidation
Copper/copper oxide and the yellowish-brown showed) the reason of limit and work continuously on site, the arrangement that factory floor can be more flexible
The production of each process section can also without being limited to after copper not store and must carry out at once the next step due to subtracting
This process section is split outsourcing, the more more options in actual production are realized.
Specific embodiment
This case is further explained and is illustrated With reference to embodiment, specifically: use different passivator
It is passivated operation to the copper foil base material after copper is subtracted, corrosion test then is carried out to the copper foil base material after Passivation Treatment, observes copper
The corrosion condition on paper tinsel base material surface, and then evaluate the anticorrosion ability of passivator.
Testing program
1) test grouping
According to the difference of passivator, it is grouped into A, B, C；
Wherein
A: subtracting copper post-processing with a kind of RTR of the present invention and obtained with the technical solution in copper foil surface passivator, and specific group
At:
Antioxidant is benzotriazole, 17g/L；
Complexing agent is disodium ethylene diamine tetraacetate, 3g/L；
Activator is fatty alcohol polyoxyethylene ether, 0.2g/L；
Solvent is dehydrated alcohol, 40g/L；
Dispersing agent be sodium tripolyphosphate, polyacrylamide mass ratio 1:1 mixture, 0.2g/L；
Rare earth metal source is nitric acid cerium salt, 0.5g/L；
Attachment reinforcing agent is butyl, 1.0g/L；
Reducing agent is sodium sulfite, 0.05g/L.
PH buffer is potassium dihydrogen phosphate-sodium hydroxide solution, takes 1.36g potassium dihydrogen phosphate, the configuration of 0.4g sodium hydroxide
At mixed solution, mixed solution mass concentration is 1.76g/L.
Remaining is pure water.
The basic passivating solution of B:15%BTA；
C: pure water；
2) passivation operation
Using the passivation mode of immersion, temperature is room temperature (25 ± 5 DEG C), and passivation time is 5 minutes.
3) nitric acid pitting test
Nitric acid spot corrosion test: (25 ± 5 DEG C) under room temperature, using the nitric acid solution of 50% volume fraction as corrosive liquid into
Concrete operations: row copper foil corrosion resistant test by corrosion drop in substrate surface, observes corrosion condition (the color change on its surface
Change), record the time of first bubble generation.
Test result
Nitric acid spot corrosion test result
4) rear surface color change situation is placed in storage
By the copper foil base material storage after Passivation Treatment, the variation (situation of change of surface color) of its surface topography is observed,
25 ± 5 DEG C of storage environment temperature, humidity≤70%.
After a week, smooth, the non-oxidation trace that subtracts copper copper foil surface after the surface treatment of above-mentioned A group passivating solution；And B group
The basic passivating solution processing copper foil base material anticorrosion time is short, and after 3 days resting periods, substrate surface can be observed with the naked eye clearly
Discoloration (brown mist evidence of corrosion)；The copper foil base material surface oxidation of C group control group is the most serious, and the resting period is less than one
It.
Copper foil base material exterior appearance corrosion condition is stored in warehouse
| Test group | Exterior appearance judgment criteria | TDiscoloration/ day |
| A | Whether copper foil surface is bright, and whether there is or not evidence of oxide | > 7 |
| B | Whether copper foil surface is bright, and whether there is or not evidence of oxide | < 3 |
| C | Whether copper foil surface is bright, and whether there is or not evidence of oxide | < 1 |
。
Claims (9)
1. a kind of RTR subtracts copper post-processing copper foil surface passivator, which is characterized in that the passivator includes mass fraction
Following substance:
Antioxidant 15-20g/L, complexing agent 3-5g/L, surfactant 0.1-0.3g/L, solvent 30-45g/L, dispersing agent
0.1-0.3g/L, rare earth metal source 0.5-1.0g/L, attachment reinforcing agent 0.8-1.2g/L, buffer, reducing agent 0.05-0.1g/
L。
2. RTR as described in claim 1 subtracts copper post-processing copper foil surface passivator, which is characterized in that antioxidant is benzene
And triazole.
3. RTR as described in claim 1 subtracts copper post-processing copper foil surface passivator, which is characterized in that complexing agent is diamines
Tetraacethyl disodium, tetrasodium ethylenediamine tetraacetate, ethylenediamine, monoethanolamine, diethanol amine, triethanolamine, ammonium sulfate, ammonium chloride,
One or more of citrate, pyrophosphate, tartrate, sulphite, thiosulfate, sodium gluconate etc..
4. RTR as described in claim 1 subtracts copper post-processing copper foil surface passivator, which is characterized in that surfactant is
One or more of fatty alcohol polyoxyethylene ether, aliphatic amine polyoxyethylene ether and castor oil phosphate ester.
5. RTR as described in claim 1 subtracts copper post-processing copper foil surface passivator, which is characterized in that rare earth metal source is
Lanthanum nitrate and/or nitric acid cerium salt.
6. RTR as described in claim 1 subtracts copper post-processing copper foil surface passivator, which is characterized in that adhering to reinforcing agent is
Monoethanolamine and/or butyl.
7. RTR as described in claim 1 subtracts copper post-processing copper foil surface passivator, which is characterized in that reducing agent is sulfurous
One or more of hydrochlorate, sodium hypophosphite, boron hydride, hydrazine hydrate etc..
8. the RTR as described in claim 1-8 any claim subtracts the preparation method of copper post-processing copper foil surface passivator,
It is characterized in that, the preparation method comprises the following steps that
A. the antioxidant of proportion mass parts is added into solvent, is thoroughly mixed uniformly；
B. the rare earth metal source salt of proportion mass parts is added into above-mentioned mixed solution；
C. the complexing agent of proportion mass parts is added into above-mentioned mixed solution, stirs evenly；
D. the activator of proportion mass parts is added into above-mentioned mixed solution, is mixed evenly；
E. the dispersing agent of proportion mass parts is added into above-mentioned mixed solution, is mixed evenly；
F. the attachment reinforcing agent of proportion mass parts is added into above-mentioned mixed solution, is mixed evenly；
G. the pH buffer solvent of proportion mass parts is added, so that solution pH value is between 6.5-7.5；
H. surplus is pure water, constant volume.
9. the RTR as described in claim 1-8 any claim subtracts the application method of copper post-processing copper foil surface passivator,
It is characterized in that, passivator completely attaches to substrate surface when using, and passivator operating temperature: 30 ± 10 DEG C, fountain, work pressure
Power: 0.8-1.2 kg/cm2, immersion type, passivator need to do not cross substrate surface.
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| CN201910479282.0A CN110195222A (en) | 2019-06-04 | 2019-06-04 | A kind of RTR subtracts copper post-processing copper foil surface passivator and its use and preparation method |
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| CN201910479282.0A CN110195222A (en) | 2019-06-04 | 2019-06-04 | A kind of RTR subtracts copper post-processing copper foil surface passivator and its use and preparation method |
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Cited By (3)
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| CN110592568A (en) * | 2019-09-16 | 2019-12-20 | 铜陵市华创新材料有限公司 | Environment-friendly anti-oxidation liquid for negative current collector and preparation and use methods thereof |
| CN111962081A (en) * | 2020-08-11 | 2020-11-20 | 湖北工程学院 | Organic phosphonic acid and derivative thereof based copper foil anti-oxidation additive and preparation method thereof |
| CN112342534A (en) * | 2020-11-11 | 2021-02-09 | 桂林漓佳金属有限责任公司 | Passivating agent for passivating copper alloy surface |
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Application publication date: 20190903 |