CN104388996A - Black hole liquid and preparation method thereof - Google Patents
Black hole liquid and preparation method thereof Download PDFInfo
- Publication number
- CN104388996A CN104388996A CN201410599132.0A CN201410599132A CN104388996A CN 104388996 A CN104388996 A CN 104388996A CN 201410599132 A CN201410599132 A CN 201410599132A CN 104388996 A CN104388996 A CN 104388996A
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- conductive carbon
- black
- sodium
- black holes
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Abstract
The invention discloses black hole liquid, comprising the following raw materials in percentage by mass: 0.5%-5% of a conductive carbon material, 0.1%-2% of a surfactant, 0.1%-0.5% of fumed silica, 0.1%-5% of a dispersing agent, 1-5% of a pH modifier and the balance of water. The black hole liquid disclosed by the invention is good in stability, and the problem of settlement in the use process can be avoided, thus the equipment is saved, the cost is saved, and the black hole liquid is non-toxic, free of pollution and friendly to the environment.
Description
Technical field
The invention belongs to printed-wiring board (PWB) field, be specifically related to a kind of black holes liquid for printed-wiring board (PWB) and preparation method thereof.
Background technology
Printed-wiring board (PWB) hole metallization technology is one of key of printing plate manufacturing technology, for a long time, people one realize straight through the method for electroless copper, but the technical process of this method is loaded down with trivial details, coating bad mechanical property, and in use easily cause environmental pollution, therefore, black holes Direct Electroplating technology is arisen at the historic moment.
Black holes method is by physical action (electrostatic adhesion), is attached to by conductive carbon powder on hole wall and forms one deck conducting film, then Direct Electroplating, replaces chemical-copper-plating process.But the performance of hole blackening solution still has deficiency at present, such as, adopt formaldehyde as reductive agent, not only endanger ecotope, also the safety of operator is produced and threaten; The stability of black holes liquid also has much room for improvement, and often needs in operation to add circulation stirring system in black holes groove, not only increases the expense of equipment, and makes manipulation become more complicated, more may have influence on the quality control of product.
Summary of the invention
For overcoming deficiency of the prior art, the invention provides a kind of black holes liquid that can be used for printed circuit board (PCB), good stability, safety and environmental protection.
For achieving the above object, technical scheme of the present invention is, a kind of black holes liquid, according to weight percent, conductive carbon material 0.5-5%, tensio-active agent 0.1-2%, aerosil 0.1-0.5%, dispersion agent 0.1-5%, pH adjusting agent 1-5%, surplus are water;
Wherein, described conductive carbon material is through the graphitized carbon black of oxidation modification and the mixture of graphite.
Wherein, described tensio-active agent is one or more in alkylphenol polyoxyethylene, isomeric alcohol polyethenoxy ether, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate.
Described dispersion agent is one or more in polyoxyethylene glycol, Weibull, sodium lignosulfonate, EDETATE SODIUM.
Described pH adjusting agent is one or more in sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood, dipotassium hydrogen phosphate, Sodium Tetraborate, sodium borohydride, POTASSIUM BOROHYDRIDE.
Described conductive carbon material is through the graphitized carbon black of oxidation modification and the mixture of graphite, and particle diameter is at 100-300nm.
One in the mixture following methods of described graphitized carbon black and graphite carries out oxidation modification:
By conductive carbon starting material, i.e. the mixture of graphitized carbon black and graphite, reflux 12 hours in concentrated nitric acid;
Or, conductive carbon starting material are stirred 24 hours in the saturated solution of ammonium persulphate;
Or, hydrogen peroxide is slowly added in the raw-material aqueous solution of conductive carbon, heat 80 degree, stir 12 hours.
The present invention also provides a kind of preparation method of black holes liquid, according to above-mentioned composition and content, prepares according to the following steps:
A. conductive carbon starting material are carried out oxidation modification process;
B. the conductive carbon material after modification and tensio-active agent, aerosil, dispersion agent, pH adjusting agent are added to the water in proportion, are heated to 60 degree, stir and obtain black holes liquid;
Described conductive carbon starting material are mixtures of graphitized carbon black and graphite.
Wherein, carry out Surface Oxidation Modification process to conductive carbon starting material, its treatment process is selected from the one in following methods:
By conductive carbon starting material reflux 12 hours in concentrated nitric acid;
Or, conductive carbon starting material are stirred 24 hours in the saturated solution of ammonium persulphate;
Or, hydrogen peroxide is slowly added in the raw-material aqueous solution of conductive carbon, heat 80 degree, stir 12 hours.
The present invention will originally be the conductive carbon starting material of hydrophobic nature, first be carried out surface modification treatment, i.e. functionalization, make it be modified as surface and have certain hydrophilic conductive carbon material, thus can better with the combination such as tensio-active agent, dispersion agent.
Black holes liquid of the present invention is made up of the denatured conductive carbon material that conductivity is extremely strong, and good stability can avoid settlement issues in use, thus the equipment of saving, cost-saving; And nontoxic, pollution-free, environmentally friendly, environmental protection.
Preparation method of the present invention is simple, easy to operate, is applicable to suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read content of the present invention, these equivalent form of values fall within limited range of the present invention equally.
Embodiment 1
| Component | Content (weight percentage) |
| The mixture of conductive carbon black and graphite | 0.5％ |
| Sodium lauryl sulphate | 0.2％ |
| Isomerous tridecanol polyoxyethylene ether | 0.2％ |
| Aerosil | 0.1％ |
| Polyoxyethylene glycol | 0.2％ |
| Sodium lignosulfonate | 0.05％ |
| Sodium hydroxide | 1.5％ |
| Water | Surplus |
This black holes liquid can stablize a not sedimentation in month.
This black holes liquid and preparation method thereof comprises the following steps:
(1) mixture of conductive carbon black and graphite is carried out oxidation modification process and obtain conductive carbon material;
(2) aerosil, dispersion agent, pH adjusting agent are added to the water in proportion to stir and obtain the first mixing solutions;
(3) add in above-mentioned mixing solutions by the conductive carbon material after functionalization, mechanical stirring evenly obtains the second mixing solutions;
(4) add a certain amount of tensio-active agent by above-mentioned second mixing solutions, heat 60 degree, stir and obtain black holes liquid.
Embodiment 2
| Component | Content (weight percentage) |
| The mixture of conductive carbon black and graphite | 2％ |
| Nonyl naphthols Soxylat A 25-7 | 0.3％ |
| Isomery ten polyoxyethylenated alcohol | 0.1％ |
| Aerosil | 0.2％ |
| Polyoxyethylene glycol | 0.15％ |
| Weibull | 0.05％ |
| Sodium lignosulfonate | 0.05％ |
| Sodium Tetraborate | 0.5％ |
| Sodium carbonate | 1.5％ |
| Water | Surplus |
This black holes liquid can stablize a not sedimentation in month.
Production method is with embodiment 1.
Embodiment 3
| Component | Content (weight percentage) |
| Conductive carbon black | 1％ |
| Graphite | 3％ |
| Polyoxyethylene octylphenol ether | 1％ |
| Sodium dodecylbenzene sulfonate | 1％ |
| Aerosil | 0.5％ |
| Polyoxyethylene glycol | 0.1％ |
| Sodium lignosulfonate | 0.05％ |
| Sodium Tetraborate | 1.5％ |
| Water | Surplus |
This black holes liquid can stablize not sedimentation in 20 days.
Embodiment 4
| Component | Content (weight percentage) |
| Conductive carbon black | 3％ |
| Graphite | 2％ |
| Sodium lauryl sulphate | 0.7％ |
| Dodecyl phenol polyethenoxy ether | 0.3％ |
| Aerosil | 0.5％ |
| EDETATE SODIUM | 3％ |
| Sodium lignosulfonate | 2％ |
| Sodium borohydride | 5％ |
| Water | Surplus |
This black holes liquid can keep not sedimentation in 40 days.
Black holes liquid of the present invention is made up of the denatured conductive carbon material that conductivity is extremely strong, and good stability can avoid settlement issues in use, thus the equipment of saving, cost-saving; And nontoxic, pollution-free, environmentally friendly, environmental protection.
Be more than the description to the embodiment of the present invention, by the above-mentioned explanation to the disclosed embodiments, professional and technical personnel in the field realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (8)
1. a black holes liquid, it is characterized in that, according to weight percent, described black holes liquid comprises: conductive carbon material 0.5-5%, tensio-active agent 0.1-2%, aerosil 0.1-0.5%, dispersion agent 0.1-5%, pH adjusting agent 1-5%, surplus are water;
Wherein, described conductive carbon material is through the graphitized carbon black of oxidation modification and the mixture of graphite.
2. black holes liquid according to claim 1, is characterized in that, described tensio-active agent is one or more in alkylphenol polyoxyethylene, isomeric alcohol polyethenoxy ether, sodium lauryl sulphate, Sodium dodecylbenzene sulfonate.
3. black holes liquid according to claim 1, is characterized in that, described dispersion agent is one or more in polyoxyethylene glycol, Weibull, sodium lignosulfonate, EDETATE SODIUM.
4. black holes liquid according to claim 1, is characterized in that, described pH adjusting agent is one or more in sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood, dipotassium hydrogen phosphate, Sodium Tetraborate, sodium borohydride, POTASSIUM BOROHYDRIDE.
5. black holes liquid according to claim 1, is characterized in that, described conductive carbon material is through the graphitized carbon black of oxidation modification and the mixture of graphite, and particle diameter is at 100-300nm.
6., according to the arbitrary described black holes liquid of Claims 1 to 5, it is characterized in that, the one in the mixture following methods of described graphitized carbon black and graphite carries out oxidation modification:
By conductive carbon starting material, i.e. the mixture of graphitized carbon black and graphite, reflux 12 hours in concentrated nitric acid;
Or, conductive carbon starting material are stirred 24 hours in the saturated solution of ammonium persulphate;
Or, hydrogen peroxide is slowly added in the raw-material aqueous solution of conductive carbon, heat 80 degree, stir 12 hours.
7. a preparation method for black holes liquid, is characterized in that, according to the composition in claim 1 ~ 6 and content, prepares according to the following steps:
A. conductive carbon starting material are carried out oxidation modification process, obtain conductive carbon material;
B. the conductive carbon material after modification and tensio-active agent, aerosil, dispersion agent, pH adjusting agent are added to the water in proportion, are heated to 60 degree, stir and obtain black holes liquid;
Described conductive carbon starting material are mixtures of graphitized carbon black and graphite.
8. the preparation method of black holes liquid according to claim 7, is characterized in that, carries out Surface Oxidation Modification process to conductive carbon starting material, and its treatment process is selected from the one in following methods:
By conductive carbon starting material reflux 12 hours in concentrated nitric acid;
Or, conductive carbon starting material are stirred 24 hours in the saturated solution of ammonium persulphate;
Or, hydrogen peroxide is slowly added in the raw-material aqueous solution of conductive carbon, heat 80 degree, stir 12 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410599132.0A CN104388996A (en) | 2014-10-30 | 2014-10-30 | Black hole liquid and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410599132.0A CN104388996A (en) | 2014-10-30 | 2014-10-30 | Black hole liquid and preparation method thereof |
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| CN104388996A true CN104388996A (en) | 2015-03-04 |
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| CN201410599132.0A Pending CN104388996A (en) | 2014-10-30 | 2014-10-30 | Black hole liquid and preparation method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818506A (en) * | 2015-05-28 | 2015-08-05 | 哈尔滨工业大学 | Solution for metalizing printed circuit board hole |
| CN105603477A (en) * | 2015-12-22 | 2016-05-25 | 苏州禾川化学技术服务有限公司 | Novel process for pretreatment of chemical copper plating of ABS (acrylonitrile butadiene styrene) plastics |
| 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 |
| 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 |
| CN108323036A (en) * | 2018-02-10 | 2018-07-24 | 深圳市祥盛兴科技有限公司 | A kind of blank hole liquid and black holes chemical industry skill |
| 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 |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4619741A (en) * | 1985-04-11 | 1986-10-28 | Olin Hunt Specialty Products Inc. | Process for preparing a non-conductive substrate for electroplating |
| US4622107A (en) * | 1986-05-05 | 1986-11-11 | Olin Hunt Specialty Products Inc. | Process for preparing the through hole walls of a printed wiring board for electroplating |
| 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 |
| CN1439451A (en) * | 2002-11-18 | 2003-09-03 | 长沙矿冶研究院 | Nano-diamond deagglomeration and grading method |
| CN1733980A (en) * | 2004-08-02 | 2006-02-15 | 吕桂生 | Electricity conductive liquid capable of directly galvanizing the printed board |
| 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 |
| CN102593413A (en) * | 2012-01-16 | 2012-07-18 | 浙江超威创元实业有限公司 | Manufacturing method of pole piece for improving current density |
| CN103160896A (en) * | 2013-03-01 | 2013-06-19 | 溧阳市新力机械铸造有限公司 | Preparing method of black hole solution for printed circuit board |
| CN103167747A (en) * | 2013-03-01 | 2013-06-19 | 溧阳市新力机械铸造有限公司 | Manufacturing method of printed circuit board |
| CN103487469A (en) * | 2013-09-29 | 2014-01-01 | 哈尔滨工业大学 | Experiment board for checking black hole process effect of printed circuit board as well as checking method |
-
2014
- 2014-10-30 CN CN201410599132.0A patent/CN104388996A/en active Pending
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4619741A (en) * | 1985-04-11 | 1986-10-28 | Olin Hunt Specialty Products Inc. | Process for preparing a non-conductive substrate for electroplating |
| US4622107A (en) * | 1986-05-05 | 1986-11-11 | Olin Hunt Specialty Products Inc. | Process for preparing the through hole walls of a printed wiring board for electroplating |
| 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 |
| CN1439451A (en) * | 2002-11-18 | 2003-09-03 | 长沙矿冶研究院 | Nano-diamond deagglomeration and grading method |
| CN1733980A (en) * | 2004-08-02 | 2006-02-15 | 吕桂生 | Electricity conductive liquid capable of directly galvanizing the printed board |
| 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 |
| CN102593413A (en) * | 2012-01-16 | 2012-07-18 | 浙江超威创元实业有限公司 | Manufacturing method of pole piece for improving current density |
| CN103160896A (en) * | 2013-03-01 | 2013-06-19 | 溧阳市新力机械铸造有限公司 | Preparing method of black hole solution for printed circuit board |
| CN103167747A (en) * | 2013-03-01 | 2013-06-19 | 溧阳市新力机械铸造有限公司 | Manufacturing method of printed circuit board |
| CN103487469A (en) * | 2013-09-29 | 2014-01-01 | 哈尔滨工业大学 | Experiment board for checking black hole process effect of printed circuit board as well as checking method |
Non-Patent Citations (1)
| Title |
|---|
| 刘天池: "印制电路工艺技术的进步", 《电子工艺技术》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104818506A (en) * | 2015-05-28 | 2015-08-05 | 哈尔滨工业大学 | Solution for metalizing printed circuit board hole |
| CN105603477A (en) * | 2015-12-22 | 2016-05-25 | 苏州禾川化学技术服务有限公司 | Novel process for pretreatment of chemical copper plating of ABS (acrylonitrile butadiene styrene) plastics |
| CN105603477B (en) * | 2015-12-22 | 2017-12-26 | 苏州禾川化学技术服务有限公司 | A kind of ABS plastic electro-coppering pretreatment process |
| 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 |
| CN106535505B (en) * | 2016-11-23 | 2019-04-02 | 昆山尚宇电子科技有限公司 | Blank hole liquid for printed board manufacture |
| 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 |
| 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 |
| CN108323036A (en) * | 2018-02-10 | 2018-07-24 | 深圳市祥盛兴科技有限公司 | A kind of blank hole liquid and black holes chemical industry skill |
| 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 |
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Application publication date: 20150304 |
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