CN103160896B - Preparing method of black hole solution for printed circuit board - Google Patents

Preparing method of black hole solution for printed circuit board Download PDF

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Publication number
CN103160896B
CN103160896B CN201310066887.XA CN201310066887A CN103160896B CN 103160896 B CN103160896 B CN 103160896B CN 201310066887 A CN201310066887 A CN 201310066887A CN 103160896 B CN103160896 B CN 103160896B
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China
Prior art keywords
solution
circuit board
printed circuit
mixing solutions
fatty alcohol
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Expired - Fee Related
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CN201310066887.XA
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CN103160896A (en
Inventor
曹小真
陈信华
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LIYANG XINLI MACHINERY CASTING CO Ltd
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LIYANG XINLI MACHINERY CASTING CO Ltd
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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

A kind of preparation method of use in printed circuit board hole blackening solution
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 up of film, has the significant superiority such as flexible structure, volume are little, lightweight, not only can static bend, and can also make Dynamic flexural, 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 solved between electronic functionalities module that appears as of printed circuit board (PCB).Rigid-flexible refers in conjunction with printed circuit board (PCB) and utilizes flexible parent metal and the printed circuit board (PCB) interconnecting in different zones and rigid substrate and make.In rigid flexible system district, the conductive pattern on flexible parent metal and rigid substrate is interconnected by plated through-hole usually.Rigid-flexible can connect the circuit between Different Plane in conjunction with printed circuit board (PCB), can fold, bend, crispatura, also can movable part connecting part, realize three dimensional wiring, thus solve the restricted problem of script in many encapsulation, improve Connection Density and reliability.In order to realize the metallization of hole wall, the method for current main employing " black holes " in the field of business realizes.
" black holes " method is by adopting hole blackening solution dipping printed circuit board (PCB), the effect utilizing positive and negative charge attracting makes the organism macromolecular material (material such as polyimide film, epoxy resin binder, acrylic resin adhesive, epoxy glass fiber cloth) of the carbon particles and hole wall with conducting function combine closely, for follow-up electro-coppering provides one deck reliable electroconductibility medium.But the performance of hole blackening solution still has deficiency at present, such as, adopt formaldehyde to make reductive agent, because the toxicity of formaldehyde is comparatively large, not only endangers ecotope, and have carcinogenic danger.The less stable of hole blackening solution, operates and careless slightlyly just there will be solution decomposes.Black holes 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
Object of the present invention is just to overcome the deficiencies in the prior art, a kind of preparation method that can be used for the hole blackening solution of printed circuit board (PCB) is provided, the hole blackening solution utilizing the method to prepare carries out plated through-hole, not only security is greatly improved, and effectively can control the quantity discharged of waste water, simplify production technique, reduce the production cost of printed board.
The preparation method of the hole blackening solution that the present invention proposes comprises the steps:
(1) by carbon dust, Na 2siO 3, NH 4after OH and water mix and blend, reflux 20 hours, obtains the first mixing solutions;
(2) in above-mentioned first mixing solutions, add anion surfactant, after mechanical stirring is even, obtain the second mixing solutions;
(3) add nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent successively at above-mentioned second mixing solutions, stir rear reflux 10 hours;
(4) to the mechanical stirring on one side of the solution after completing steps (3), naturally cool to normal temperature, obtain hole blackening solution.
Wherein, be 100 parts by weight with the hole blackening solution finally completed, 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, pareth sulfate;
Nonionogenic tenside is: polysorbate, fatty alcohol-polyoxyethylene ether.Fatty alcohol in described fatty alcohol-polyoxyethylene ether is: carbonatoms is the fatty alcohol of 10-20.
Negatively charged ion non-ionic composite tensio-active agent contains at least Liang Ge functional group, 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, such as: polyoxyethylene ether sulfate, Soxylat A 25-7 soap.
Embodiment:
Below by embodiment, the preparation method to the hole blackening solution that the present invention proposes is described in detail.
Embodiment 1
The preparation method of the hole blackening solution that the present invention proposes comprises the steps:
(1) by carbon dust, Na 2siO 3, NH 4after OH and water mix and blend, reflux 20 hours, obtains the first mixing solutions;
(2) in above-mentioned first mixing solutions, add anion surfactant, after mechanical stirring is even, obtain the second mixing solutions;
(3) add nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent successively at above-mentioned second mixing solutions, stir rear reflux 10 hours;
(4) to the mechanical stirring on one side of the solution after completing steps (3), naturally cool to normal temperature, obtain hole blackening solution.
Wherein, be 100 parts by weight with the hole blackening solution finally completed, 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, pareth sulfate;
Nonionogenic tenside is: polysorbate, fatty alcohol-polyoxyethylene ether.Fatty alcohol in described fatty alcohol-polyoxyethylene ether is: carbonatoms is the fatty alcohol of 10-20.
Negatively charged ion non-ionic composite tensio-active agent contains at least Liang Ge functional group, 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, such as: polyoxyethylene ether sulfate, Soxylat A 25-7 soap.
Embodiment 2
List the preferred embodiment of the hole blackening solution preparation method that the present invention proposes below,
The preparation method of the hole blackening solution that the present invention proposes comprises the steps:
(1) by carbon dust, Na 2siO 3, NH 4after OH and water mix and blend, reflux 20 hours, obtains the first mixing solutions;
(2) in above-mentioned first mixing solutions, add anion surfactant, after mechanical stirring is even, obtain the second mixing solutions;
(3) add nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent successively at above-mentioned second mixing solutions, stir rear reflux 10 hours;
(4) to the mechanical stirring on one side of the solution after completing steps (3), naturally cool to normal temperature, obtain hole blackening solution.
Wherein, be 100 parts by weight with the hole blackening solution finally completed, 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 to invention has been detailed introduction, but above-mentioned embodiment is not intended to limit scope of the present invention, and protection scope of the present invention is defined by the appended claims.

Claims (2)

1. a preparation method for use in printed circuit board hole blackening solution, is characterized in that comprising the steps:
(1) by carbon dust, Na 2siO 3, NH 4after OH and water mix and blend, reflux 20 hours, obtains the first mixing solutions;
(2) in above-mentioned first mixing solutions, add anion surfactant, after mechanical stirring is even, obtain the second mixing solutions;
(3) add nonionogenic tenside and negatively charged ion non-ionic composite tensio-active agent successively at above-mentioned second mixing solutions, stir rear reflux 10 hours;
(4) to the mechanical stirring on one side of the solution after completing steps (3), naturally cool to normal temperature, obtain hole blackening solution;
Wherein, be 100 parts by weight with the hole blackening solution finally completed, 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%.
2. the preparation method of 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, pareth sulfate;
Described nonionogenic tenside is: polysorbate, fatty alcohol-polyoxyethylene ether; Fatty alcohol in described fatty alcohol-polyoxyethylene ether is: carbonatoms is the fatty alcohol of 10-20;
Described negatively charged ion non-ionic composite tensio-active agent contains at least Liang Ge functional group, and 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.
CN201310066887.XA 2013-03-01 2013-03-01 Preparing method of black hole solution for printed circuit board Expired - Fee Related CN103160896B (en)

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Families Citing this family (4)

* Cited by examiner, † Cited by third party
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
CN109825863B (en) * 2019-03-28 2021-02-05 烟台恒诺新材料有限公司 Application of carbon nano tube conductive paste in black hole direct electroplating

Citations (5)

* Cited by examiner, † Cited by third party
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
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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