CN106191952A - A kind of black holes liquid and methods for making and using same thereof - Google Patents
A kind of black holes liquid and methods for making and using same thereof Download PDFInfo
- Publication number
- CN106191952A CN106191952A CN201610572976.5A CN201610572976A CN106191952A CN 106191952 A CN106191952 A CN 106191952A CN 201610572976 A CN201610572976 A CN 201610572976A CN 106191952 A CN106191952 A CN 106191952A
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- CN
- China
- Prior art keywords
- black holes
- liquid
- holes liquid
- resin
- black
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Classifications
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/12—Semiconductors
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
Abstract
The invention discloses a kind of black holes liquid and methods for making and using same thereof, this black holes liquid include 0.1% 1% nano silver wire, the surfactant of 0.1% 5%, the dispersant of 1% 3%, the PH regulator of 1% 5%, the resin of 1% 5%, the hydroxymethyl cellulose of 1% 2%, the levelling agent of 1% 3%, the carrier solvent of 78% 90%.Being all to need through modified or special handling, complex process due to white carbon black, graphite or even the CNT in general black holes liquid, the present invention is then to be made into water-base cement simply, and preparation is simple.Secondly when apply in printed circuit board field, the electric conductivity of nano silver wire is relatively good, and a small amount of application (0.1 1%) can keep good electric conductivity, is conducive to lifting speed and cost-effective.The most also will not produce heavy metal pollution, environmental-protecting performance is good, has preferable market application foreground.
Description
Technical field
The present invention relates to printed substrate technical field, particularly relate to a kind of black holes liquid and preparation thereof and application side
Method.
Background technology
Printed substrate hole metallization technology is one of key of printed panel manufacturing technology, and for a long time, people one are led directly to
The method crossing electroless copper realizes, but the technological process of this method is loaded down with trivial details, coating bad mechanical property, and in use holds
Easily causing environmental pollution, therefore, black holes Direct Electroplating technology is arisen at the historic moment.
Black holes method is by physical action (Electrostatic Absorption), is attached to conductive carbon powder on hole wall form one layer of conduction
Film, then Direct Electroplating, replace chemical-copper-plating process.But the conductive carbon material in general black holes liquid is through modified and special
The different white carbon black processed and graphite, complex process during preparation, and long flow path.And white carbon black and graphite in blank hole liquid are it is generally required to relatively
High solid content (such as 10%), and sheet resistance is higher, monolithic conductive is poor, and observable index is higher, the most long.
Therefore, the present inventor needs a kind of new technique of design badly to improve its problem.
Summary of the invention
It is desirable to provide a kind of black holes liquid and methods for making and using same thereof, its solution allocation is convenient, electric conductivity
Getting well and will not produce heavy metal, environmental-protecting performance is good.
For solving above-mentioned technical problem, the technical scheme is that
A kind of black holes liquid, including the component of following percentage by weight:
Preferably, one or more during described carrier solvent is aqueous isopropanol, aqueous solution, ethanol solution.
Preferably, a length of 10-40 μm of described nano silver wire, a diameter of 20-80nm.
Preferably, described resin is propylene glycol methyl ether acetate, ethyl cellosolve acetate, TDI modified alkyd resin, contains
One or more of vinyl chloride-vinyl acetate resin and acrylic resin.
Preferably, described PH regulator be the one in sodium hydroxide, potassium hydroxide, sodium carbonate, dipotassium hydrogen phosphate or
Multiple.
Preferably, described dispersant be triethyl group hexyl phosphoric acid, sodium lauryl sulphate, methyl anyl alcohol, cellulose derive
One or more in thing, polyacrylamide, guar gum, fatty acid polyethylene glycol ester.
Preferably, described surfactant is alkylphenol polyoxyethylene, isomeric alcohol polyethenoxy ether, lauryl sulphate acid
One or more in sodium, dodecylbenzene sodium sulfonate.
The preparation method of a kind of black holes liquid as described above, comprises the steps:
S1: proportionally by nano silver wire, surfactant, dispersant, PH regulator, resin, aerosil, hydroxyl
Methylcellulose, levelling agent add in carrier solvent, mix homogeneously；
S2: be heated to more than 50 DEG C, is uniformly mixing to obtain this black holes liquid.
The application process of a kind of black holes liquid, comprises the steps:
ST1: printed circuit board (PCB) is carried out；
ST2: printed circuit board (PCB) is carried out black holes process；
The black holes liquid used in wherein said black holes processing procedure is according to formula described above or preparation method
It is prepared from.
Preferably, described step ST2 carries out black holes process by impregnated or horizontal to printed circuit board (PCB).
Using technique scheme, the present invention at least includes following beneficial effect:
It is all to need through modified or special handling due to white carbon black, graphite or even the CNT in general black holes liquid
, and black holes liquid of the present invention and methods for making and using same thereof, then it is to be made into water-base cement simply, configuration side
Just.Secondly the electric conductivity of nano silver wire is relatively good, and a small amount of application (0.1-1%) can keep good electric conductivity, is conducive to
The speed of follow-up electro-coppering and cost-effective.The most also will not produce heavy metal pollution, environmental-protecting performance is good, has preferably
Market application foreground.
Detailed description of the invention
Below by way of specific instantiation, embodiments of the present invention being described, those skilled in the art can be by this specification
Disclosed content understands other advantages and effect of the present invention easily.The present invention can also be by the most different concrete realities
The mode of executing is carried out or applies, the every details in this specification can also based on different viewpoints and application, without departing from
Various modification or change is carried out under the spirit of the present invention.Enclose.
A kind of black holes liquid, including the component of following percentage by weight:
Preferably, table 1 is seen, including below embodiment:
Table 1
Preferably, one or more during described carrier solvent is aqueous isopropanol, aqueous solution, ethanol solution.
Preferably, a length of 10-40 μm of described nano silver wire, a diameter of 20-80nm.Most preferably, described silver is received
A length of 30 μm of rice noodle, a diameter of 50nm.
Preferably, described resin is propylene glycol methyl ether acetate, ethyl cellosolve acetate, TDI modified alkyd resin, contains
One or more of vinyl chloride-vinyl acetate resin and acrylic resin.
Preferably, described PH regulator be the one in sodium hydroxide, potassium hydroxide, sodium carbonate, dipotassium hydrogen phosphate or
Multiple.
Preferably, described dispersant be triethyl group hexyl phosphoric acid, sodium lauryl sulphate, methyl anyl alcohol, cellulose derive
One or more in thing, polyacrylamide, guar gum, fatty acid polyethylene glycol ester.
Preferably, described surfactant is alkylphenol polyoxyethylene, isomeric alcohol polyethenoxy ether, lauryl sulphate acid
One or more in sodium, dodecylbenzene sodium sulfonate.
Heretofore described levelling agent preferably includes following component:
Butyl acrylate 5-10 part,
Siloxane-Oxyalkylene Copolymers 3-9 part,
Tetrasodium pyrophosphate 2-7 part,
Sodium chloride 3-7 part,
Bamboo powder 4-9 part,
Curing polyester resin 2-7 part,
Epoxy resin 3-9 part.
This levelling agent has preferable levelability and decoration performance, accelerates and the volatilization of balanced solvent, can reduce life simultaneously
Absorption to dust during product, improves the releasability of solvent, promotes levelling and feel.
In a preferred embodiment, described resin is preferably TDI modified alkyd resin, and it is in terms of drying property and hardness
Relatively ordinary resin is significantly improved, and surface drying time shortens to 30min from 5-6h, and the time of doing solid work shortens to 4h from 15-18h, significantly
Improve efficiency.
In a preferred embodiment, described resin is preferably vinyl chloride-vinyl acetate resin and acrylic resin, owing to the molecule of the two is
Straight-chain, during solidification, cubical contraction is relatively big, and the spacing of nano silver wire diminishes, and sheet resistance is relatively low.
In a preferred embodiment, described resin is preferably polyurethane and epoxy resin, containing more formation hydrogen in the two
Bond polarity group, surface electrostatic gravitation and intermolecular force are bigger, and resin bonding is best, prepared black holes liquid
Tack is good.
The preparation method of a kind of black holes liquid as described above, comprises the steps:
S1: proportionally by nano silver wire, surfactant, dispersant, PH regulator, resin, aerosil, hydroxyl
Methylcellulose, levelling agent add in carrier solvent, mix homogeneously；
S2: be heated to more than 50 DEG C, is uniformly mixing to obtain this black holes liquid.
The application process of a kind of black holes liquid, comprises the steps:
ST1: printed circuit board (PCB) is carried out；
ST2: printed circuit board (PCB) is carried out black holes process；
The black holes liquid used in wherein said black holes processing procedure is according to formula described above or preparation method
It is prepared from.
Certainly, this printed circuit board (PCB) also needs to carry out subsequent treatment, as cleaned, being dried, the operation such as copper facing, owing to it is
Routine techniques means of the prior art, therefore here is omitted.
Preferably, described step ST2 carries out black holes process by impregnated or horizontal to printed circuit board (PCB).Due to
Impregnated and horizontal this area skill personnel know, therefore here is omitted.
Owing to nano silver wire is easily dispersed in isopropanol, aqueous solution, the dispersion that ethanol solution also can be suitable, the most preferably locate
Reason liquid is aqueous solution.In view of the low content of nano silver wire, therefore in treatment fluid, the content of resin or polymer should be lower,
Between 1-5%, it is to avoid too much embedding nano silver wire and non-conductive after causing cured later.(the hydroxylmethyl cellulose of about 1%
Element, has thickening power, provides the bonding force with printed substrate after solidification).
The experiment effect of the present invention can be proved by following contrast experiment:
Sample 1a, the black holes liquid described in embodiment 1.
Sample 1b, the black holes liquid described in embodiment 2.
Sample 1c, the black holes liquid described in embodiment 3.
Sample 2, a kind of black holes liquid, comprise conductive carbon material 0.5-5%, surfactant 0.1-2%, gas phase titanium dioxide
Silicon 0.1-0.5%, dispersant 0.1-5%, pH adjusting agent 1-5%, surplus are water.Wherein, described conductive carbon material is through peroxide
Change modified conductive black and the mixture of graphite.
Sample 3, a kind of blank hole liquid for printed circuit board, including conductive matrices, surfactant, water soluble polymer
And the poor solvent of correspondence, alkaline matter, disperse medium, organic solvent, defoamer, inorganic bond.Wherein said conduction
Substrate is 2-5 part；Described surfactant is 0.8-1.2 part；The poor solvent of described water soluble polymer and correspondence thereof is respectively
For 1-2 part and 15-25 part；Described alkaline matter is 2-4 part；Described disperse medium is 50-70 part, the organic solvent of 8-12 part,
The defoamer of 0.4-1.0 part, the inorganic bond of 0.5-1.5 part.
Sample 4, a kind of black holes liquid, comprise CNT, surfactant, alkaline matter and appropriate liquid flux.
Wherein, CNT, after functionalization, is stably scattered in this hole blackening solution under the effect of dispersant.
Sample 1-4 is respectively used to printed circuit board (PCB), and experimental result sees table 2.
Table 2
| Sedimentation time | Residual degree | Whether containing defoamer | Bubble with or without | Sheet resistance | |
| Sample 1a | 90 days | 80% | No | Nothing | 100 ohm/cm |
| Sample 1b | 100 days | 84% | No | Nothing | 88 ohm/cm |
| Sample 1c | 120 days | 86% | No | Nothing | 90 ohm/cm |
| Sample 2 | One month | 62% | It is | Nothing | 150 ohm/cm |
| Sample 3 | 20 days | 62% | No | Have | 150 ohm/cm |
| Sample 4 | 45 days | 67% | No | Have | 200 ohm/cm |
By above-mentioned contrast test, we it appeared that the sedimentation time of black holes liquid of the present invention apparently higher than it
His sample, stability is higher.Additionally sheet resistance is relatively low, and electric energy loss is less, and electric conductivity is good.What is more important without
Defoamer, still will not produce bubble, save production cost while improving product presentation quality on surface.
And the configuration of the black holes liquid of the present invention is more convenient, white carbon black in general black holes liquid, graphite, CNT are all
Being to need through modified and special handling, the present invention is then to be made into water-base cement simply, secondly the electric conductivity of nano silver wire
Relatively good, a small amount of application (0.1-1%) can keep good electric conductivity, the speed of follow-up electro-coppering and saving
Cost.And comprise white carbon black, graphite, CNT blank hole liquid it is generally required to higher solid content (such as 10%), and its surface
Resistance is higher, and overall electric conductivity is poor, and observable index is higher, the most long.Additionally the present invention also will not produce heavy metal
Polluting, environmental-protecting performance is good, has preferable market application foreground.
Described above to the disclosed embodiments, makes professional and technical personnel in the field be capable of or uses the present invention.
Multiple amendment to these embodiments will be apparent from for those skilled in the art, as defined herein
General Principle can realize without departing from the spirit or scope of the present invention in other embodiments.Therefore, the present invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and principles disclosed herein and features of novelty phase one
The widest scope caused.
Claims (10)
1. a black holes liquid, it is characterised in that include the component of following percentage by weight:
Nano silver wire 0.1%-1%；
Surfactant 0.1%-5%；
Dispersant 1%-3%；
PH regulator 1%-5%；
Resin 1%-5%；
Hydroxymethyl cellulose 1%-2%；
Levelling agent 1%-3%；
Carrier solvent 78%-90%.
2. black holes liquid as claimed in claim 1, it is characterised in that: described carrier solvent is aqueous isopropanol, aqueous solution, second
One or more in alcoholic solution.
3. black holes liquid as claimed in claim 1 or 2, it is characterised in that: a length of 10-40 μm of described nano silver wire, directly
Footpath is 20-80nm.
4. the black holes liquid as described in claim 1-3 is arbitrary, it is characterised in that: described resin be propylene glycol methyl ether acetate,
Ethyl cellosolve acetate, TDI modified alkyd resin, containing one or more of vinyl chloride-vinyl acetate resin and acrylic resin.
5. the black holes liquid as described in claim 1-4 is arbitrary, it is characterised in that: described PH regulator is sodium hydroxide, hydrogen-oxygen
Change in potassium, sodium carbonate, dipotassium hydrogen phosphate one or more.
6. the black holes liquid as described in claim 1-5 is arbitrary, it is characterised in that: described dispersant be triethyl group hexyl phosphoric acid,
In sodium lauryl sulphate, methyl anyl alcohol, cellulose derivative, polyacrylamide, guar gum, fatty acid polyethylene glycol ester one
Plant or multiple.
7. the black holes liquid as described in claim 1-6 is arbitrary, it is characterised in that: described surfactant is alkyl phenol polyoxy second
One or more in alkene ether, isomeric alcohol polyethenoxy ether, sodium lauryl sulphate, dodecylbenzene sodium sulfonate.
8. the preparation method of the black holes liquid as described in claim 1-7 is arbitrary, it is characterised in that comprise the steps:
S1: proportionally by nano silver wire, surfactant, dispersant, PH regulator, resin, aerosil, methylol
Cellulose, levelling agent add in carrier solvent, mix homogeneously；
S2: be heated to more than 50 DEG C, is uniformly mixing to obtain this black holes liquid.
9. the application process of a black holes liquid, it is characterised in that comprise the steps:
ST1: printed circuit board (PCB) is carried out；
ST2: printed circuit board (PCB) is carried out black holes process；
The black holes liquid used in wherein said black holes processing procedure is according to the arbitrary described formula of claim 1-7 or power
Profit requires that the preparation method described in 8 is prepared from.
10. the application process of black holes liquid as claimed in claim 9, it is characterised in that: described step ST2 passes through impregnated
Or horizontal carries out black holes process to printed circuit board (PCB).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610572976.5A CN106191952A (en) | 2016-07-20 | 2016-07-20 | A kind of black holes liquid and methods for making and using same thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610572976.5A CN106191952A (en) | 2016-07-20 | 2016-07-20 | A kind of black holes liquid and methods for making and using same thereof |
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| CN106191952A true CN106191952A (en) | 2016-12-07 |
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| CN201610572976.5A Pending CN106191952A (en) | 2016-07-20 | 2016-07-20 | A kind of black holes liquid and methods for making and using same thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107740145A (en) * | 2017-10-16 | 2018-02-27 | 广州市天承化工有限公司 | A kind of highly conductive carbon pores liquid of pcb board and its preparation method and application |
| CN109825863A (en) * | 2019-03-28 | 2019-05-31 | 烟台恒诺新材料有限公司 | A kind of carbon nanotube conducting starches the application in black holesization is directly electroplated |
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| CN104021840A (en) * | 2014-06-18 | 2014-09-03 | 中南大学 | Low-temperature curing high-conductive silver paste, preparation method of low-temperature curing high-conductive silver paste, conductive film and preparation method of conductive film |
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| CN105419444A (en) * | 2015-12-23 | 2016-03-23 | 苏州创科微电子材料有限公司 | Nano silver wire electric-conductive glue and electroplating method |
| CN105702323A (en) * | 2016-03-15 | 2016-06-22 | 张家港瑞诺光电材料科技有限公司 | Flexible conductive silver paste and manufacturing method |
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2016
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107740145A (en) * | 2017-10-16 | 2018-02-27 | 广州市天承化工有限公司 | A kind of highly conductive carbon pores liquid of pcb board and its preparation method and application |
| CN109825863A (en) * | 2019-03-28 | 2019-05-31 | 烟台恒诺新材料有限公司 | A kind of carbon nanotube conducting starches the application in black holesization is directly electroplated |
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Application publication date: 20161207 |