CN108323036A - A kind of blank hole liquid and black holes chemical industry skill - Google Patents
A kind of blank hole liquid and black holes chemical industry skill Download PDFInfo
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- CN108323036A CN108323036A CN201810137389.2A CN201810137389A CN108323036A CN 108323036 A CN108323036 A CN 108323036A CN 201810137389 A CN201810137389 A CN 201810137389A CN 108323036 A CN108323036 A CN 108323036A
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- wiring board
- blank hole
- printed wiring
- black
- hole liquid
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Classifications
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
- H05K3/42—Plated through-holes or plated via connections
- H05K3/423—Plated through-holes or plated via connections characterised by electroplating method
- H05K3/424—Plated through-holes or plated via connections characterised by electroplating method by direct electroplating
-
- 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
-
- 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
- H05K2203/00—Indexing scheme relating to apparatus or processes for manufacturing printed circuits covered by H05K3/00
- H05K2203/07—Treatments involving liquids, e.g. plating, rinsing
- H05K2203/0779—Treatments involving liquids, e.g. plating, rinsing characterised by the specific liquids involved
Abstract
The invention belongs to printed wiring board technical fields, and in particular to a kind of blank hole liquid and black holes chemical industry skill.Blank hole liquid provided by the invention, including following components and its mass percent:Conductive agent 2 4%, dispersant 5 9%, surfactant 4 7%, potassium carbonate 1 2%, deionized water 78 88%.For blank hole liquid provided by the invention without chemical compositions such as EDTA, NTA, EDTP, the feature of environmental protection is good, has the characteristics that polymolecularity, high stability, wetability are good, permeability is good, has good long-time stability and performance.In addition, black holes chemical industry skill simple operation provided by the invention.
Description
Technical field
The invention belongs to printed wiring board technical fields, and in particular to a kind of blank hole liquid and black holes chemical industry skill.
Background technology
Printed wiring board (PCB, FPC) hole metallization technology is the key that one of printed board manufacturing technology, for a long time, people
Use electroless copper plating (PTH) always method, but various chemical substances containing harmful ecological environment in PTH solution, such as
EDTA, NTA, EDTP and easy carcinogenic formaldehyde, wastewater treatment is complicated, of high cost;In addition, PTH stabilities of solution are poor, it is molten
Complexity is safeguarded in the analysis of liquid;The mechanical performance of PTH copper plates is poor simultaneously, and technological process is cumbersome, therefore industry is being sought always
It is exactly to come into being in this background to look for new hole metallization technology, the direct electroplating technology of black holesization.
Black holes is that fine graphite and carbon black powder dip-coating are formed conductive layer on hole wall, is then directly electroplated.
Its key technology is exactly the composition of black holes solution composition.Fine graphite and carbon black powder are uniformly dispersed in medium first
I.e. in deionized water, equally distributed graphite and carbon black granules in solution are made to keep stablizing using the surfactant in solution,
There is good wettability simultaneously, graphite and carbon black is enable fully to be attracted on idioelectric hole wall surface, formed uniform
Conductive layer that is careful, being firmly combined with.
Chinese patent application CN106319604A discloses a kind of black holes formula of liquid, including following components:Conductive matrices divide
Dispersion media, surfactant, dispersant, alkaline matter.The dispersant suitably matched, dispersant are added in the formula of the invention
Being adsorbed on surface of the conductive matrix improves the hydrophily of conductive matrices, and effect suspension stabilization is not susceptible to coagulation, black holes has been effectively ensured
The performance of liquid.But the conductive matrices in the invention are nano-sized carbon, long-time stability need to be further increased.China
Patent CN704562775B discloses a kind of blank hole liquid and preparation method thereof for printed circuit board, and blank hole liquid includes conductive base
Matter, surfactant, water soluble polymer and its corresponding poor solvent, alkaline matter and decentralized medium, the preparation of blank hole liquid
Method includes that conductive matrices, surfactant are added in decentralized medium, water soluble polymer is added after being ground, acutely
The corresponding poor solvent of water soluble polymer is added after stirring, is finally added alkaline matter and is formed blank hole liquid.Though the invention
So enhance the dispersion stabilization of blank hole liquid, still, by be added in black hole fluid water soluble polymer and its it is corresponding not
Good solvent forms the blank hole liquid of the conductive matrices of hydrophilic polymer cladding, conductive matrices meeting after water soluble polymer coats
Influence the electric conductivity of conductive matrices.
Existing blank hole liquid is the suspension that conductive matrices (carbon black, graphite particle) is made using water as decentralized medium, due to
The hydrophily of conductive matrices is poor, causes suspension unstable, coagulation easily occurs, and has seriously affected the performance of blank hole liquid.
Although more in relation to the research for improving stability of suspension, still lack one kind in the prior art and takes into account stability and use
The blank hole liquid of performance.
Invention content
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of blank hole liquid and black holes chemical industry skills.The present invention
For the blank hole liquid of offer without chemical compositions such as EDTA, NTA, EDTP, the feature of environmental protection is good, has polymolecularity, high stability, wetability
Well, the features such as permeability is good has good long-time stability and performance.In addition, black holes chemical industry provided by the invention
Skill simple operation.
The technical scheme is that:
A kind of blank hole liquid, including following components and its mass percent:Conductive agent 2-4%, dispersant 5-9%, surface are lived
Property agent 4-7%, potassium carbonate 1-2%, deionized water 78-88%.
Further, the blank hole liquid is made of following components and its mass percent:Conductive agent 2.5%, dispersant
6.5%, surfactant 6%, potassium carbonate 1.5%, deionized water 83.5%.
Further, the conductive agent is by acetylene black, conductive black and graphene 1-3 in mass ratio:2-5:9-12 is formed.
Further, the conductive agent is by acetylene black, conductive black and graphene in mass ratio 2:3:10 compositions.
Further, the dispersant is by polyvinyl alcohol, polycarboxylate and polyacrylamide 1-3 in mass ratio:3-6:8-
10 compositions.
Further, the dispersant is by polyvinyl alcohol, polycarboxylate and polyacrylamide in mass ratio 2:5:9 groups
At.
Further, the surfactant presses matter by sorbitan monostearate and thermally coupled distillation columns
Amount compares 3-5:9-11 is formed.
Further, the surfactant is pressed by sorbitan monostearate and thermally coupled distillation columns
Mass ratio 4:10 compositions.
The preparation method of the blank hole liquid is:
(1) surfactant is add to deionized water, is stirred evenly, obtain dispersion liquid A;
(2) dispersant is added in dispersion liquid A obtained by step (1), stirs evenly, obtains dispersion liquid B;
(3) conductive agent is added in dispersion liquid B obtained by step (2), sonic oscillation 7-10min, supersonic frequency 40-
60KHz obtains dispersion liquid C;
(4) potassium carbonate is added in dispersion liquid C obtained by step (3), grinding, milling time be 2.5-4h to get.
In addition the present invention also provides black holes chemical industry skill, include the following steps:
S1 cleans whole hole processing:At room temperature, printed wiring board is put into after impregnating 1-3min in alkalescent detergent and is taken out,
It is rinsed with water totally, then, the printed wiring board after water is rinsed, which is put into regulator, impregnates 60-80s, must clean whole hole processing
Printed wiring board afterwards;
S2 water cleans:Printed wiring board is rinsed with water totally after whole hole processing will be cleaned obtained by step S1, after obtaining water cleaning
Printed wiring board;
The processing of S3 black holesization:At room temperature, printed wiring board after water cleaning obtained by step S2 is put into blank hole liquid and impregnates 60-
150s obtains printed wiring board after black holesization processing;
S4 water cleans:Printed wiring board after black holesization processing obtained by step S3 is rinsed with water totally, clean track is obtained
Road plate;
S5 is dried:At a temperature of 80 DEG C, clean printed wiring board obtained by step S4 is air-dried, printed wiring after must drying
Plate;
The processing of S6 microetches:At room temperature, printed wiring board, which is put into micro-etching agent, after will be dry obtained by step S5 impregnates 90-150s
After take out, be then rinsed with water clean, be dried;
Blank hole liquid described in step S3 is blank hole liquid of the present invention.
Blank hole liquid provided by the invention by acetylene black, conductive black and graphene by certain mass than form conductive agent,
By polyvinyl alcohol, polycarboxylate and polyacrylamide by certain mass than form dispersant, by sorbitan monostearate and
Surfactant, potassium carbonate and deionized water of the thermally coupled distillation columns by certain mass than composition form.This
The blank hole liquid that invention provides is using deionized water as decentralized medium, collaboration of the conductive agent therein in dispersant, surfactant etc.
Under effect so that the stability of blank hole liquid enhances, and is not susceptible to coagulation, and with polymolecularity, high stability, wetability is good, oozes
The features such as permeability is good has both good performance while with good long-time stability.
In black holes chemical industry skill of the present invention, step S1 cleans the effect of whole hole processing:Conductive agent is with negative in hole blackening solution
Charge, the negatively charged mutually repulsion of hole wall resin surface institute with after drilling, is unable to Electrostatic Absorption, directly affects the absorption of conductive agent
Effect.By adjusting the adjusting that agent is positively charged, the negative electrical charge of resin surface institute band can be neutralized or even hole wall can also be assigned
Resin positive charge, in order to adsorb conductive agent.
In black holes chemical industry skill of the present invention, the step S2, effect of S4 water cleaning:Clean the Liquid Residue with excess surface in hole.
In black holes chemical industry skill of the present invention, the effect of step S3 black holesization processing:By physisorption, make hole wall base material
One layer of uniform and delicate of adsorption conductive layer.
In black holes chemical industry skill of the present invention, the effect of step S5 dryings:Remove adsorption layer contained humidity, with promote conductive agent with
Adhesive force between hole wall substrate surface.
In black holes chemical industry skill of the present invention, the effect of step S6 microetches processing:It is handled first with micro-etching agent, conductive layer is made to present
Microswelling generates micro channel.This is because during black holes, conductive agent is not only attracted on hole wall, but also is inhaled
It is attached in the surface layers of copper of internal layer copper ring and substrate, to ensure that electro-coppering and matrix copper have good combination, it is necessary to will be on copper
Conductive agent removes.Only have conductive layer to generate micro channel thus, can just be etched liquid removing.Because micro-etching agent is generated by conductive layer
Micro channel etch to layers of copper, and copper face microetch is made to fall 1-2 μm, the conductive agent on copper is made to be removed due to without place is based oneself upon,
And the conductive agent on hole wall non-conductor substrate keeps original state, and good conductive layer is provided for directly plating.
Compared with prior art, the present invention has the advantage that:
(1) blank hole liquid provided by the invention is free of traditional electroless copper ingredient, and formaldehyde and harm are not used in formula
The chemical substance of ecological environment such as EDTA, NTA, EDTP etc., belong to environmentally friendly machine.
(2) blank hole liquid provided by the invention has the characteristics that polymolecularity, high stability, wetability are good, permeability is good, tool
There are good long-time stability and performance.
(3) black holes chemical industry skill process simplification provided by the invention, instead of very thin and uncontrollable middle layer (chemical plating
Layers of copper), so as to improve the adhesive force of electro-coppering, improve the reliability of PCB/FPC hole metallizations.
(4) present invention significantly simplifies the analysis of solution, maintenance and management uses program.
(5) compared with traditional PTH, simple operation of the present invention is with short production cycle, and waste disposal fee is reduced, to drop
The totle drilling cost of low production.
Specific implementation mode
The following describes the present invention further through the description of specific embodiments, but this is not the limit to the present invention
System, those skilled in the art's basic thought according to the present invention can make various modifications or improvements, but without departing from this
The basic thought of invention, is all within the scope of the present invention.
In the present invention, polycarboxylate is purchased from Ju Te Science and Technology Ltd.s of Shenzhen, model:JUST-1860;Polyvinyl alcohol
It is purchased from the good Chemical Industry Science Co., Ltd of Shanghai fond dream, model:Powder;Polyacrylamide is purchased from Gongyi City
Yuan Tong water-purifying materials Co., Ltd, model:ytpam;Alkalescent detergent is purchased from hundred Shi Lu lubricating oil Co., Ltd of Shenzhen,
Model:Castrol Techniclean S-RP;Micro-etching agent is purchased from Shenzhen Run Sun Chemical Technology Co., Ltd., model:RS-
855W。
Embodiment 1, a kind of blank hole liquid
The blank hole liquid is made of following components and its mass percent:Conductive agent 2%, dispersant 5%, surfactant
4%, potassium carbonate 1%, deionized water 88%;The conductive agent is by acetylene black, conductive black and graphene in mass ratio 1:5:12
Composition;The dispersant is by polyvinyl alcohol, polycarboxylate and polyacrylamide in mass ratio 1:6:10 compositions;The surface-active
Agent is by sorbitan monostearate and thermally coupled distillation columns in mass ratio 3:11 compositions.
The preparation method of the blank hole liquid is:
(1) surfactant is add to deionized water, is stirred evenly, obtain dispersion liquid A;
(2) dispersant is added in dispersion liquid A obtained by step (1), stirs evenly, obtains dispersion liquid B;
(3) conductive agent is added in dispersion liquid B obtained by step (2), sonic oscillation 7min, supersonic frequency 40KHz are obtained
Dispersion liquid C;
(4) potassium carbonate is added in dispersion liquid C obtained by step (3), grinding, milling time be 2.5h to get.
Black holes chemical industry skill, includes the following steps:
S1 cleans whole hole processing:At room temperature, printed wiring board is put into after impregnating 1min in alkalescent detergent and is taken out, used
Water is rinsed well, and then, the printed wiring board after water is rinsed, which is put into regulator, impregnates 60s, is printed after must cleaning whole hole processing
Wiring board processed;
S2 water cleans:Printed wiring board is rinsed with water totally after whole hole processing will be cleaned obtained by step S1, after obtaining water cleaning
Printed wiring board;
The processing of S3 black holesization:At room temperature, printed wiring board after water cleaning obtained by step S2 is put into blank hole liquid and is impregnated
60s obtains printed wiring board after black holesization processing;
S4 water cleans:Printed wiring board after black holesization processing obtained by step S3 is rinsed with water totally, clean track is obtained
Road plate;
S5 is dried:At a temperature of 80 DEG C, clean printed wiring board obtained by step S4 is air-dried, printed wiring after must drying
Plate;
The processing of S6 microetches:At room temperature, will it is dry obtained by step S5 after printed wiring board be put into impregnate 90s in micro-etching agent after take
Go out, is then rinsed with water totally, is dried.
Embodiment 2, a kind of blank hole liquid
The blank hole liquid is made of following components and its mass percent:Conductive agent 4%, dispersant 9%, surfactant
7%, potassium carbonate 2%, deionized water 78%;The conductive agent is by acetylene black, conductive black and graphene in mass ratio 3:5:12
Composition;The dispersant is by polyvinyl alcohol, polycarboxylate and polyacrylamide in mass ratio 3:6:10 compositions;The surface-active
Agent is by sorbitan monostearate and thermally coupled distillation columns in mass ratio 5:11 compositions.
The preparation method of the blank hole liquid is:
(1) surfactant is add to deionized water, is stirred evenly, obtain dispersion liquid A;
(2) dispersant is added in dispersion liquid A obtained by step (1), stirs evenly, obtains dispersion liquid B;
(3) conductive agent is added in dispersion liquid B obtained by step (2), sonic oscillation 10min, supersonic frequency 60KHz,
Obtain dispersion liquid C;
(4) potassium carbonate is added in dispersion liquid C obtained by step (3), grinding, milling time be 4h to get.
Black holes chemical industry skill, includes the following steps:
S1 cleans whole hole processing:At room temperature, printed wiring board is put into after impregnating 3min in alkalescent detergent and is taken out, used
Water is rinsed well, and then, the printed wiring board after water is rinsed, which is put into regulator, impregnates 80s, is printed after must cleaning whole hole processing
Wiring board processed;
S2 water cleans:Printed wiring board is rinsed with water totally after whole hole processing will be cleaned obtained by step S1, after obtaining water cleaning
Printed wiring board;
The processing of S3 black holesization:At room temperature, printed wiring board after water cleaning obtained by step S2 is put into blank hole liquid and is impregnated
150s obtains printed wiring board after black holesization processing;
S4 water cleans:Printed wiring board after black holesization processing obtained by step S3 is rinsed with water totally, clean track is obtained
Road plate;
S5 is dried:At a temperature of 80 DEG C, clean printed wiring board obtained by step S4 is air-dried, printed wiring after must drying
Plate;
The processing of S6 microetches:At room temperature, will it is dry obtained by step S5 after after printed wiring board is put into and impregnates 150s in micro-etching agent
It takes out, is then rinsed with water totally, is dried.
Embodiment 3, a kind of blank hole liquid
The blank hole liquid is made of following components and its mass percent:Conductive agent 2.5%, dispersant 6.5%, surface are lived
Property agent 6%, potassium carbonate 1.5%, deionized water 83.5%;The conductive agent presses quality by acetylene black, conductive black and graphene
Than 2:3:10 compositions;The dispersant is by polyvinyl alcohol, polycarboxylate and polyacrylamide in mass ratio 2:5:9 compositions;It is described
Surfactant is by sorbitan monostearate and thermally coupled distillation columns in mass ratio 4:10 compositions.
The preparation method of the blank hole liquid is:
(1) surfactant is add to deionized water, is stirred evenly, obtain dispersion liquid A;
(2) dispersant is added in dispersion liquid A obtained by step (1), stirs evenly, obtains dispersion liquid B;
(3) conductive agent is added in dispersion liquid B obtained by step (2), sonic oscillation 8min, supersonic frequency 50KHz are obtained
Dispersion liquid C;
(4) potassium carbonate is added in dispersion liquid C obtained by step (3), grinding, milling time be 3h to get.
Black holes chemical industry skill, includes the following steps:
S1 cleans whole hole processing:At room temperature, printed wiring board is put into after impregnating 2min in alkalescent detergent and is taken out, used
Water is rinsed well, and then, the printed wiring board after water is rinsed, which is put into regulator, impregnates 70s, is printed after must cleaning whole hole processing
Wiring board processed;
S2 water cleans:Printed wiring board is rinsed with water totally after whole hole processing will be cleaned obtained by step S1, after obtaining water cleaning
Printed wiring board;
The processing of S3 black holesization:At room temperature, printed wiring board after water cleaning obtained by step S2 is put into blank hole liquid and is impregnated
110s obtains printed wiring board after black holesization processing;
S4 water cleans:Printed wiring board after black holesization processing obtained by step S3 is rinsed with water totally, clean track is obtained
Road plate;
S5 is dried:At a temperature of 80 DEG C, clean printed wiring board obtained by step S4 is air-dried, printed wiring after must drying
Plate;
The processing of S6 microetches:At room temperature, will it is dry obtained by step S5 after after printed wiring board is put into and impregnates 120s in micro-etching agent
It takes out, is then rinsed with water totally, is dried.
Comparative example 1, a kind of blank hole liquid
The blank hole liquid is made of following components and its mass percent:Conductive agent 2.5%, dispersant 6.5%, surface are lived
Property agent 6%, potassium carbonate 1.5%, deionized water 83.5%;The conductive agent presses quality by acetylene black, conductive black and graphene
Than 1:1:1 composition;The dispersant is by polyvinyl alcohol, polycarboxylate and polyacrylamide in mass ratio 2:5:9 compositions;The table
Face activating agent is by sorbitan monostearate and thermally coupled distillation columns in mass ratio 4:10 compositions.
Preparation method, the black holes chemical industry skill of the blank hole liquid are similar to Example 3.
Difference lies in the conductive agent is by acetylene black, conductive black and graphene in mass ratio 1 with embodiment 3:1:1
Composition.
Comparative example 2, a kind of blank hole liquid
The blank hole liquid is made of following components and its mass percent:Conductive agent 2.5%, dispersant 6.5%, surface are lived
Property agent 6%, potassium carbonate 1.5%, deionized water 83.5%;The conductive agent presses quality by acetylene black, conductive black and graphene
Than 2:3:10 compositions;The dispersant is by polyvinyl alcohol, polycarboxylate and polyacrylamide in mass ratio 2:5:9 compositions;It is described
Surfactant is by sorbitan monostearate and thermally coupled distillation columns in mass ratio 4:10 compositions.
The black holes chemical industry skill is similar to Example 3.
Difference lies in step (4) milling time is 5h in the preparation method of the blank hole liquid with embodiment 3.Comparative example
3, a kind of blank hole liquid
The blank hole liquid is made of following components and its mass percent:Conductive agent 2.5%, dispersant 6.5%, surface are lived
Property agent 6%, potassium carbonate 1.5%, deionized water 83.5%;The conductive agent presses quality by acetylene black, conductive black and graphene
Than 2:3:10 compositions;The dispersant is by polyvinyl alcohol, polycarboxylate and polyacrylamide in mass ratio 1:1:1 composition;It is described
Surfactant is by sorbitan monostearate and thermally coupled distillation columns in mass ratio 4:10 compositions.
Preparation method, the black holes chemical industry skill of the blank hole liquid are similar to Example 3.
With embodiment 3 difference lies in, the dispersants by polyvinyl alcohol, polycarboxylate and polyacrylamide in mass ratio
1:1:1 composition.
Comparative example 4, a kind of blank hole liquid
The blank hole liquid is made of following components and its mass percent:Conductive agent 2.5%, dispersant 6.5%, surface are lived
Property agent 6%, potassium carbonate 1.5%, deionized water 83.5%;The conductive agent presses quality by acetylene black, conductive black and graphene
Than 2:3:10 compositions;The dispersant is by polycarboxylate and polyacrylamide in mass ratio 5:9 compositions;The surfactant by
Sorbitan monostearate and thermally coupled distillation columns in mass ratio 4:10 compositions.
Preparation method, the black holes chemical industry skill of the blank hole liquid are similar to Example 3.
Difference lies in the dispersant is by polycarboxylate and polyacrylamide in mass ratio 5 with embodiment 3:9 compositions.
Comparative example 5, a kind of blank hole liquid
The blank hole liquid is made of following components and its mass percent:Conductive agent 2.5%, dispersant 6.5%, surface are lived
Property agent 6%, potassium carbonate 1.5%, deionized water 83.5%;The conductive agent presses quality by acetylene black, conductive black and graphene
Than 2:3:10 compositions;The dispersant is by polyvinyl alcohol, polycarboxylate and polyacrylamide in mass ratio 2:5:9 compositions;It is described
Surfactant is by sorbitan monostearate and thermally coupled distillation columns in mass ratio 1:1 composition.
Preparation method, the black holes chemical industry skill of the blank hole liquid are similar to Example 3.
Difference lies in the surfactant is by sorbitan monostearate and Nonyl pheno with embodiment 3
Ether phosphate in mass ratio 1:1 composition.
Test example one, centrifugal stability experiment
1, test material:Embodiment 1, embodiment 2, embodiment 3, comparative example 2, comparative example 3, comparative example 4, comparative example 5 are made
The blank hole liquid obtained.
2, test method:
20mL embodiments 1, embodiment 2, embodiment 3, comparative example 2, comparative example 3, comparative example 4, comparative example 5 is measured respectively to make
It is m that the blank hole liquid obtained, which is put into quality,lCentrifuge tube in, the quality for weighing blank hole liquid and centrifuge tube is m2.By equipped with blank hole liquid from
Heart pipe is put into centrifuge, and 30min is centrifuged under the speed of 4000r/min, and centrifugation liquid in pipe is poured out, centrifuge tube and pipe are weighed
The interior quality m for centrifuging the solid left3, calculate the sedimentation rate of blank hole liquid, sedimentation rate=(m3-ml)/(m2-ml) × 100%.
3, test result:Test result is as shown in table 1.
Table 1:Centrifugal stability test result
As can be seen from Table 1, embodiment 1, embodiment 2, the sedimentation rate of blank hole liquid made from embodiment 3 are respectively
1.45%, 1.28%, 0.88%, this illustrates that blank hole liquid produced by the present invention is with good stability, wherein embodiment 3
Stability is the most excellent, is highly preferred embodiment of the present invention;Compared with comparative example 2-5,3 stability of embodiment is more preferably.
Test example two, long-term stable experiment
1, test material:Embodiment 1, embodiment 2, embodiment 3, comparative example 2, comparative example 3, comparative example 4, comparative example 5 are made
The blank hole liquid obtained.
2, test method:
Observe embodiment 1, embodiment 2, embodiment 3, comparative example 2, comparative example 3, comparative example 4, black holes made from comparative example 5
Whether there is or not laminations in 140 days for liquid.
3, test result is as shown in table 2.
Table 2:Long-term stable experiment result
As can be seen from Table 2, blank hole liquid made from embodiment 1 is storing 120 days layereds, black holes made from embodiment 2
Liquid is storing 130 days layereds, and in 140 days lamination does not occur for blank hole liquid made from embodiment 3, this illustrates system of the present invention
The blank hole liquid obtained has good long-time stability, wherein the stability of embodiment 3 is the most excellent, for the best reality of the present invention
Apply example;Compared with comparative example 2-5, the long-time stability of embodiment 3 are more preferably.
Test example three, performance test
Printed circuit board is used to the embodiment of the present invention 3, comparative example 1, comparative example 2, comparative example 3, comparative example 4, right respectively
Blank hole liquid made from ratio 5 after being tested according to black holes chemical industry skill provided by the invention, carries out conventional plating, to what is obtained
Sample carries out backlight detection, and the results are shown in Table 3.
Table 3:Backlight testing result
Project | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 |
Backlight level | 10 | 7 | 6 | 7 | 5 | 6 |
As can be seen from Table 3, the backlight level of 3 printed circuit board of the embodiment of the present invention is 10, this illustrates printed circuit board
After blank hole liquid produced by the present invention and black holes chemical industry skill are tested, conventional plating, obtained product backlight level are carried out
Height, this illustrates that the present invention has good copper facing effect, it is good to reflect black holes effect of the present invention indirectly;Compared with comparative example 1-5,
The backlight level higher of embodiment 3.
Claims (9)
1. a kind of blank hole liquid, which is characterized in that including following components and its mass percent:
Conductive agent 2-4%, dispersant 5-9%, surfactant 4-7%, potassium carbonate 1-2%, deionized water 78-88%.
2. blank hole liquid as described in claim 1, which is characterized in that be made of following components and its mass percent:Conductive agent
2.5%, dispersant 6.5%, surfactant 6%, potassium carbonate 1.5%, deionized water 83.5%.
3. blank hole liquid as claimed in claim 1 or 2, which is characterized in that the conductive agent is by acetylene black, conductive black and graphite
Alkene 1-3 in mass ratio:2-5:9-12 is formed.
4. blank hole liquid as claimed in claim 3, which is characterized in that the conductive agent is by acetylene black, conductive black and graphene
In mass ratio 2:3:10 compositions.
5. blank hole liquid as claimed in claim 1 or 2, which is characterized in that the dispersant is by polyvinyl alcohol, polycarboxylate and gathers
Acrylamide 1-3 in mass ratio:3-6:8-10 is formed.
6. blank hole liquid as claimed in claim 5, which is characterized in that the dispersant is by polyvinyl alcohol, polycarboxylate and poly- third
Acrylamide in mass ratio 2:5:9 compositions.
7. blank hole liquid as claimed in claim 1 or 2, which is characterized in that the surfactant is by sorbitan monostearate
With thermally coupled distillation columns 3-5 in mass ratio:9-11 is formed.
8. blank hole liquid as claimed in claim 7, which is characterized in that the surfactant is by sorbitan monostearate and nonyl
Base phenol polyethenoxy ether phosphate in mass ratio 4:10 compositions.
9. a kind of black holes chemical industry skill, which is characterized in that include the following steps:
S1 cleans whole hole processing:At room temperature, printed wiring board is put into after impregnating 1-3min in alkalescent detergent and is taken out, use water
It rinses well, then, the printed wiring board after water is rinsed, which is put into regulator, impregnates 60-80s, is printed after must cleaning whole hole processing
Wiring board processed;
S2 water cleans:Printed wiring board is rinsed with water totally after whole hole processing will be cleaned obtained by step S1, is printed after obtaining water cleaning
Wiring board;
The processing of S3 black holesization:At room temperature, printed wiring board after water cleaning obtained by step S2 is put into blank hole liquid and impregnates 60-
150s obtains printed wiring board after black holesization processing;
S4 water cleans:Printed wiring board after black holesization processing obtained by step S3 is rinsed with water totally, clean printed wiring board is obtained;
S5 is dried:At a temperature of 80 DEG C, clean printed wiring board obtained by step S4 is air-dried, printed wiring board after must drying;
The processing of S6 microetches:At room temperature, will it is dry obtained by step S5 after printed wiring board be put into impregnate 90-150s in micro-etching agent after take
Go out, is then rinsed with water totally, is dried;
Blank hole liquid described in step S3 is claim 1-8 any one of them blank hole liquids.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN201810137389.2A CN108323036A (en) | 2018-02-10 | 2018-02-10 | A kind of blank hole liquid and black holes chemical industry skill |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108834309A (en) * | 2018-08-30 | 2018-11-16 | 陈伟元 | A kind of graphene metallization solution and the preparation method and application thereof |
CN109811382A (en) * | 2019-03-28 | 2019-05-28 | 烟台恒诺新材料有限公司 | A kind of application of graphene oxide conductive paste in black holesization is directly electroplated |
CN111647901A (en) * | 2020-05-15 | 2020-09-11 | 湖北省哈福生物化学有限公司 | Black hole liquid and preparation method and use method thereof |
CN113207243A (en) * | 2021-05-08 | 2021-08-03 | 电子科技大学中山学院 | Preparation and application method of black hole liquid |
CN114245613A (en) * | 2021-11-30 | 2022-03-25 | 武汉格智新材料有限公司 | Carbon black pore solution, preparation method thereof and black pore process |
CN115594171A (en) * | 2022-07-29 | 2023-01-13 | 广东利尔化学有限公司(Cn) | Carbon pore process nano graphite dispersion liquid and preparation method thereof |
CN115594171B (en) * | 2022-07-29 | 2024-04-30 | 广东利尔化学有限公司 | Carbon pore process nano graphite dispersion liquid and preparation method thereof |
Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1063395A (en) * | 1991-01-10 | 1992-08-05 | 机械电子工业部第十五研究所 | The non-chemical plating hole metallizing process-hole blackening method |
US5389270A (en) * | 1993-05-17 | 1995-02-14 | Electrochemicals, Inc. | Composition and process for preparing a non-conductive substrate for electroplating |
CN101394712A (en) * | 2007-09-21 | 2009-03-25 | 清华大学 | Hole blackening solution and preparation thereof |
CN103103590A (en) * | 2013-01-08 | 2013-05-15 | 西北工业大学 | Direct-electroplating conductive liquid and preparation method thereof |
CN104388996A (en) * | 2014-10-30 | 2015-03-04 | 苏州禾川化学技术服务有限公司 | Black hole liquid and preparation method thereof |
CN104562115A (en) * | 2014-07-04 | 2015-04-29 | 广东丹邦科技有限公司 | Black hole liquid for printed circuit board and preparation method of black hole liquid |
CN105063681A (en) * | 2015-08-28 | 2015-11-18 | 韶关硕成化工有限公司 | High-concentration carbon hole solution for PCB and preparation method thereof |
CN105132962A (en) * | 2015-08-28 | 2015-12-09 | 韶关硕成化工有限公司 | High-concentration carbon pore solution applied to PCB boards and preparation method thereof |
CN106319604A (en) * | 2016-08-29 | 2017-01-11 | 苏州铱诺化学材料有限公司 | Blackhole solution formula |
CN106535505A (en) * | 2016-11-23 | 2017-03-22 | 昆山尚宇电子科技有限公司 | Black hole solution for manufacturing printed board |
CN107645829A (en) * | 2017-10-16 | 2018-01-30 | 广州市天承化工有限公司 | A kind of circuit board conductive liquid and its preparation method and application |
-
2018
- 2018-02-10 CN CN201810137389.2A patent/CN108323036A/en active Pending
Patent Citations (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1063395A (en) * | 1991-01-10 | 1992-08-05 | 机械电子工业部第十五研究所 | The non-chemical plating hole metallizing process-hole blackening method |
US5389270A (en) * | 1993-05-17 | 1995-02-14 | Electrochemicals, Inc. | Composition and process for preparing a non-conductive substrate for electroplating |
CN101394712A (en) * | 2007-09-21 | 2009-03-25 | 清华大学 | Hole blackening solution and preparation thereof |
CN103103590A (en) * | 2013-01-08 | 2013-05-15 | 西北工业大学 | Direct-electroplating conductive liquid and preparation method thereof |
CN104562115A (en) * | 2014-07-04 | 2015-04-29 | 广东丹邦科技有限公司 | Black hole liquid for printed circuit board and preparation method of black hole liquid |
CN104388996A (en) * | 2014-10-30 | 2015-03-04 | 苏州禾川化学技术服务有限公司 | Black hole liquid and preparation method thereof |
CN105063681A (en) * | 2015-08-28 | 2015-11-18 | 韶关硕成化工有限公司 | High-concentration carbon hole solution for PCB and preparation method thereof |
CN105132962A (en) * | 2015-08-28 | 2015-12-09 | 韶关硕成化工有限公司 | High-concentration carbon pore solution applied to PCB boards and preparation method thereof |
CN106319604A (en) * | 2016-08-29 | 2017-01-11 | 苏州铱诺化学材料有限公司 | Blackhole solution formula |
CN106535505A (en) * | 2016-11-23 | 2017-03-22 | 昆山尚宇电子科技有限公司 | Black hole solution for manufacturing printed board |
CN107645829A (en) * | 2017-10-16 | 2018-01-30 | 广州市天承化工有限公司 | A kind of circuit board conductive liquid and its preparation method and application |
Non-Patent Citations (3)
Title |
---|
代洋洋: "PCB用黑孔液组成及其制备的研究", 《中国优秀硕士学位论文全文数据库-信息科技辑》 * |
蔡积庆: "印制板黑孔化电镀工艺", 《电子工艺技术》 * |
遇世友,李宁,谢金平: "以石墨为导电基质的黑孔化新技术", 《印制电路信息》 * |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108834309A (en) * | 2018-08-30 | 2018-11-16 | 陈伟元 | A kind of graphene metallization solution and the preparation method and application thereof |
CN109811382A (en) * | 2019-03-28 | 2019-05-28 | 烟台恒诺新材料有限公司 | A kind of application of graphene oxide conductive paste in black holesization is directly electroplated |
CN109811382B (en) * | 2019-03-28 | 2021-04-20 | 烟台恒诺新材料有限公司 | Application of graphene oxide conductive paste in black hole direct electroplating |
CN111647901A (en) * | 2020-05-15 | 2020-09-11 | 湖北省哈福生物化学有限公司 | Black hole liquid and preparation method and use method thereof |
CN111647901B (en) * | 2020-05-15 | 2023-08-25 | 湖北省哈福生物化学有限公司 | Black hole liquid and preparation method and application method thereof |
CN113207243A (en) * | 2021-05-08 | 2021-08-03 | 电子科技大学中山学院 | Preparation and application method of black hole liquid |
CN114245613A (en) * | 2021-11-30 | 2022-03-25 | 武汉格智新材料有限公司 | Carbon black pore solution, preparation method thereof and black pore process |
CN115594171A (en) * | 2022-07-29 | 2023-01-13 | 广东利尔化学有限公司(Cn) | Carbon pore process nano graphite dispersion liquid and preparation method thereof |
CN115594171B (en) * | 2022-07-29 | 2024-04-30 | 广东利尔化学有限公司 | Carbon pore process nano graphite dispersion liquid and preparation method thereof |
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