CN103160896A - Preparing method of black hole solution for printed circuit board - Google Patents
Preparing method of black hole solution for printed circuit board Download PDFInfo
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- CN103160896A CN103160896A CN201310066887XA CN201310066887A CN103160896A CN 103160896 A CN103160896 A CN 103160896A CN 201310066887X A CN201310066887X A CN 201310066887XA CN 201310066887 A CN201310066887 A CN 201310066887A CN 103160896 A CN103160896 A CN 103160896A
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- solution
- circuit board
- printed circuit
- mixing solutions
- blackening solution
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Abstract
The invention discloses a preparing method of black hole solution for a printed circuit board. The preparing method comprises the following steps: (1) enabling carbon dust, Na2SiO3, NH4OH and water to be mixed, stirred and heated for 20 hours in a reflux mode to obtain first mixed solution; (2) adding negative ion surface active agents to the first mixed solution to obtain second mixed solution after mechanically even stirring; (3) successively adding non-ion surface active agents and negative-ion and non-ion composite surface active agents to the second mixed solution, and enabling the solution to be heated for 10 hours after even stirring; and (4) mechanically stirring the solution after the step (3), and enabling the solution to be cooled to normal temperature naturally to obtain black hole solution.
Description
Technical field
The invention belongs to field of printed circuit board fabrication, relate in particular to a kind of preparation method of use in printed circuit board hole blackening solution.
Background technology
Flexible printed circuit board is made of film, has the significant superiority such as flexible structure, volume are little, lightweight, not only can static deflection, can also do dynamic deflection, curling and folding.Along with the continuous fast development of printed circuit board (PCB) (PCB) processing technology, rigid-flexible provides a kind of new solution in conjunction with the interconnection problems that solves between the electronic functionalities module that appears as of printed circuit board (PCB).The printed circuit board (PCB) that rigid-flexible refers to utilize flexible parent metal and makes in different zones and rigid substrate interconnection in conjunction with printed circuit board (PCB).In hard and soft land, the conductive pattern on flexible parent metal and rigid substrate interconnects by plated through-hole usually.Rigid-flexible can connect circuit between Different Plane in conjunction with printed circuit board (PCB), can fold, crooked, crispatura, also can movable part connecting spare, realize three dimensional wiring, thereby solved the restricted problem of script in many encapsulation, improved Connection Density and reliability.In order to realize the metallization of hole wall, the method for main employing in the field of business at present " black hole " realizes.
" black hole " method is by adopting hole blackening solution dipping printed circuit board (PCB), the carbon particles that utilizes effect that positive and negative charge is inhaled mutually to make to have conducting function and the organism macromolecular material (materials such as polyimide film, epoxy resin binder, acrylic resin adhesive, epoxy glass fiber cloth) of hole wall are combined closely, for follow-up electro-coppering provides one deck reliable electroconductibility medium.But the performance of hole blackening solution still has deficiency at present, for example adopts formaldehyde to make reductive agent, because the toxicity of formaldehyde is larger, not only endangers ecotope, and carcinogenic danger is arranged.The less stable of hole blackening solution operates the careless slightly solution that will occur and decomposes.Black hole metallization processes long flow path, operation and maintenance is extremely inconvenient, and quality control is more difficult and working cost is high.
Summary of the invention
Purpose of the present invention just is to overcome the deficiencies in the prior art, a kind of preparation method who can be used for the hole blackening solution of printed circuit board (PCB) is provided, utilize the hole blackening solution that the method prepares to carry out plated through-hole, not only security is greatly improved, and can effectively control the quantity discharged of waste water, simplify production technique, reduced the production cost of printed board.
The preparation method of the hole blackening solution that the present invention proposes comprises the steps:
(1) with carbon dust, Na
2SiO
3, NH
4After OH and water mix and blend, reflux is 20 hours, obtains the first mixing solutions;
(2) add anion surfactant in above-mentioned the first mixing solutions, obtain the second mixing solutions after mechanical stirring is even;
(3) add successively nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent at above-mentioned the second mixing solutions, stir rear reflux 10 hours;
(4) to the mechanical stirring on one side of the solution after completing steps (3), Yi Bian naturally cool to normal temperature, obtain hole blackening solution.
Wherein, take the hole blackening solution finally completed as 100 weight parts, in step (1), carbon dust, Na
2SiO
3, NH
4The weight percent of OH and water is respectively: carbon dust: 2-4%, Na
2SiO
3: 0.5-1%, NH
4OH:3-4% and water: 88-93%.
Wherein, in step (2), the weight percent of anion surfactant is: 0.5-2%
Wherein, in step (3), the weight percent of nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent is respectively: 0.5-1%, 0.5-1.5%.
Wherein, anion surfactant is: one or more in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, polyoxyethylenated alcohol sodium sulfate, alkyl polyoxyethylene ether sodium sulfate;
Nonionogenic tenside is: polysorbate, fatty alcohol-polyoxyethylene ether.Fatty Alcohol(C12-C14 and C12-C18) in described fatty alcohol-polyoxyethylene ether is: carbonatoms is the Fatty Alcohol(C12-C14 and C12-C18) of 10-20.
Negatively charged ion non-ionic composite tensio-active agent contains at least two functional groups, described functional group is selected from one or more in hydroxyl (OH), carboxyl (COOH), carbon-carbon double bond (C=C), epoxide group, itrile group (CN), sulfonic group, for example: polyoxyethylene ether sulfate, Soxylat A 25-7 soap.
Embodiment:
Preparation method to the hole blackening solution of the present invention's proposition is elaborated below by embodiment.
Embodiment 1
The preparation method of the hole blackening solution that the present invention proposes comprises the steps:
(1) with carbon dust, Na
2SiO
3, NH
4After OH and water mix and blend, reflux is 20 hours, obtains the first mixing solutions;
(2) add anion surfactant in above-mentioned the first mixing solutions, obtain the second mixing solutions after mechanical stirring is even;
(3) add successively nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent at above-mentioned the second mixing solutions, stir rear reflux 10 hours;
(4) to the mechanical stirring on one side of the solution after completing steps (3), Yi Bian naturally cool to normal temperature, obtain hole blackening solution.
Wherein, take the hole blackening solution finally completed as 100 weight parts, in step (1), carbon dust, Na
2SiO
3, NH
4The weight percent of OH and water is respectively: carbon dust: 2-4%, Na
2SiO
3: 0.5-1%, NH
4OH:3-4% and water: 88-93%.
Wherein, in step (2), the weight percent of anion surfactant is: 0.5-2%;
Wherein, in step (3), the weight percent of nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent is respectively: 0.5-1%, 0.5-1.5%.
Wherein, anion surfactant is: one or more in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, polyoxyethylenated alcohol sodium sulfate, alkyl polyoxyethylene ether sodium sulfate;
Nonionogenic tenside is: polysorbate, fatty alcohol-polyoxyethylene ether.Fatty Alcohol(C12-C14 and C12-C18) in described fatty alcohol-polyoxyethylene ether is: carbonatoms is the Fatty Alcohol(C12-C14 and C12-C18) of 10-20.
Negatively charged ion non-ionic composite tensio-active agent contains at least two functional groups, described functional group is selected from one or more in hydroxyl (OH), carboxyl (COOH), carbon-carbon double bond (C=C), epoxide group, itrile group (CN), sulfonic group, for example: polyoxyethylene ether sulfate, Soxylat A 25-7 soap.
Embodiment 2
The below lists the hole blackening solution preparation method's of the present invention's proposition preferred embodiment,
The preparation method of the hole blackening solution that the present invention proposes comprises the steps:
(1) with carbon dust, Na
2SiO
3, NH
4After OH and water mix and blend, reflux is 20 hours, obtains the first mixing solutions;
(2) add anion surfactant in above-mentioned the first mixing solutions, obtain the second mixing solutions after mechanical stirring is even;
(3) add successively nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent at above-mentioned the second mixing solutions, stir rear reflux 10 hours;
(4) to the mechanical stirring on one side of the solution after completing steps (3), Yi Bian naturally cool to normal temperature, obtain hole blackening solution.
Wherein, take the hole blackening solution finally completed as 100 weight parts, in step (1), carbon dust, Na
2SiO
3, NH
4The weight percent of OH and water is respectively: carbon dust: 3%, Na
2SiO
3: 0.8%, NH
4OH:3.5% and water: 89.9%.
Wherein, in step (2), the weight percent of anion surfactant is: 1%;
Wherein, in step (3), the weight percent of nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent is respectively: 0.8% and 1%;
Wherein, anion surfactant is: sodium lauryl sulphate;
Nonionogenic tenside is: polysorbate.
Negatively charged ion non-ionic composite tensio-active agent is polyoxyethylene ether sulfate or Soxylat A 25-7 soap.
Above embodiment is described in detail the present invention, but above-mentioned embodiment is not in order to limit scope of the present invention, and protection scope of the present invention is defined by the appended claims.
Claims (3)
1. the preparation method of a use in printed circuit board hole blackening solution, is characterized in that comprising the steps:
(1) with carbon dust, Na
2SiO
3, NH
4After OH and water mix and blend, reflux is 20 hours, obtains the first mixing solutions;
(2) add anion surfactant in above-mentioned the first mixing solutions, obtain the second mixing solutions after mechanical stirring is even;
(3) add successively nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent at above-mentioned the second mixing solutions, stir rear reflux 10 hours;
(4) to the mechanical stirring on one side of the solution after completing steps (3), Yi Bian naturally cool to normal temperature, obtain hole blackening solution.
2. the preparation method of use in printed circuit board hole blackening solution as claimed in claim 1 is characterized in that:
Wherein, take the hole blackening solution finally completed as 100 weight parts, in step (1), carbon dust, Na
2SiO
3, NH
4The weight percent of OH and water is respectively: carbon dust: 2-4%, Na
2SiO
3: 0.5-1%, NH
4OH:3-4% and water: 88-93%; In step (2), the weight percent of anion surfactant is: 0.5-2%; In step (3), the weight percent of nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent is respectively: 0.5-1%, 0.5-1.5%.
3. use in printed circuit board hole blackening solution as claimed in claim 1 is characterized in that:
Wherein, described anion surfactant is: one or more in sodium lauryl sulphate, Sodium dodecylbenzene sulfonate, polyoxyethylenated alcohol sodium sulfate, alkyl polyoxyethylene ether sodium sulfate;
Described nonionogenic tenside is: polysorbate, fatty alcohol-polyoxyethylene ether.Fatty Alcohol(C12-C14 and C12-C18) in described fatty alcohol-polyoxyethylene ether is: carbonatoms is the Fatty Alcohol(C12-C14 and C12-C18) of 10-20.
Described negatively charged ion non-ionic composite tensio-active agent contains at least two functional groups, described functional group is selected from one or more in hydroxyl (OH), carboxyl (COOH), carbon-carbon double bond (C=C), epoxide group, itrile group (CN), sulfonic group, for example: polyoxyethylene ether sulfate, Soxylat A 25-7 soap.
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CN201310066887.XA CN103160896B (en) | 2013-03-01 | 2013-03-01 | Preparing method of black hole solution for printed circuit board |
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CN201310066887.XA CN103160896B (en) | 2013-03-01 | 2013-03-01 | Preparing method of black hole solution for printed circuit board |
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CN103160896A true CN103160896A (en) | 2013-06-19 |
CN103160896B CN103160896B (en) | 2015-06-10 |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN106521593A (en) * | 2016-09-05 | 2017-03-22 | 同健(惠阳)电子有限公司 | High-activity reagent for black-hole process of printed circuit board and method for black-hole process |
CN109152239A (en) * | 2017-06-28 | 2019-01-04 | 聂菲菲 | A kind of preparation method of printed circuit board hole blackening solution |
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 |
Citations (5)
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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 |
JPH0558229B2 (en) * | 1984-08-27 | 1993-08-26 | Japan Storage Battery Co Ltd | |
CN101113388A (en) * | 2006-07-28 | 2008-01-30 | 比亚迪股份有限公司 | Black-hole carbon powder cleaning agent composition and cleaning method thereof |
CN101394712A (en) * | 2007-09-21 | 2009-03-25 | 清华大学 | Hole blackening solution and preparation thereof |
CN101453837B (en) * | 2007-11-28 | 2011-03-30 | 比亚迪股份有限公司 | Hole electricity conduction method for printed circuit board |
-
2013
- 2013-03-01 CN CN201310066887.XA patent/CN103160896B/en not_active Expired - Fee Related
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH0558229B2 (en) * | 1984-08-27 | 1993-08-26 | Japan Storage Battery Co Ltd | |
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 |
CN101113388A (en) * | 2006-07-28 | 2008-01-30 | 比亚迪股份有限公司 | Black-hole carbon powder cleaning agent composition and cleaning method thereof |
CN101394712A (en) * | 2007-09-21 | 2009-03-25 | 清华大学 | Hole blackening solution and preparation thereof |
US8440158B2 (en) * | 2007-09-21 | 2013-05-14 | Tsinghua University | Pre-plating solutions for making printed circuit boards and methods for preparing the same |
CN101453837B (en) * | 2007-11-28 | 2011-03-30 | 比亚迪股份有限公司 | Hole electricity conduction method for printed circuit board |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
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 |
CN106521593A (en) * | 2016-09-05 | 2017-03-22 | 同健(惠阳)电子有限公司 | High-activity reagent for black-hole process of printed circuit board and method for black-hole process |
CN109152239A (en) * | 2017-06-28 | 2019-01-04 | 聂菲菲 | A kind of preparation method of printed circuit board hole blackening solution |
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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CN103160896B (en) | 2015-06-10 |
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Granted publication date: 20150610 Termination date: 20160301 |