CN105063681A - High-concentration carbon hole solution for PCB and preparation method thereof - Google Patents

High-concentration carbon hole solution for PCB and preparation method thereof Download PDF

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Publication number
CN105063681A
CN105063681A CN201510546799.9A CN201510546799A CN105063681A CN 105063681 A CN105063681 A CN 105063681A CN 201510546799 A CN201510546799 A CN 201510546799A CN 105063681 A CN105063681 A CN 105063681A
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China
Prior art keywords
pcb board
high density
agent
pores liquid
density carbon
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CN201510546799.9A
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Chinese (zh)
Inventor
王祥松
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Shaoguan Shuo Cheng Chemical Co Ltd
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Shaoguan Shuo Cheng Chemical Co Ltd
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Priority to CN201510546799.9A priority Critical patent/CN105063681A/en
Publication of CN105063681A publication Critical patent/CN105063681A/en
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Abstract

The invention discloses a high-concentration carbon hole solution for a PCB and a preparation method thereof. The finally obtained high-concentration carbon hole solution for the PCB comprises, by weight, 7-9% of conductive carbon materials, 4-8% of surface active agents, 4-8% of organic dispersing agents, 1-5% of wetting agents, pH conditioning agents and the balance water; the use amount of the pH conditioning agents enables the pH value of the high-concentration carbon hole solution for the PCB to be adjusted to 9.5-10.5. The high-concentration carbon hole solution is quite high in conductivity, good in stability and high in effective concentration, and avoids the settling problem in the using process; moreover, the frequency of replacing bath solutions is reduced, and the high-concentration carbon hole solution is nontoxic, free of pollution and environmentally friendly.

Description

High density carbon pores liquid of pcb board and preparation method thereof
Technical field
The invention belongs to the hole metallization field of electroplating industry, be specifically related to a kind of high density carbon pores liquid for pcb board and preparation method thereof.
Background technology
Traditional pcb board hole metallization has come mainly through electroless copper, and its technical process is loaded down with trivial details, uses tin palladium colloid in process, make copper facing process expensive, and this technological process can cause environmental pollution, and therefore, carbon pores electroplating technology arises at the historic moment.
Carbon pores Direct Electroplating technology is the copper-plated a kind of novel process of substituted chemistry.The carbon dust that its use conductive capability is stronger or graphite are as electro-conductive material.Be characterized in simplifying the technique of hole metallization, save man-hour, reduce the consumption of material and effectively control the quantity discharged of waste water, reduce the production cost of pcb board.
But, along with people to product to go more and more higher, its composition and the requirement of aspect of performance also more and more higher.The particularly increase of aperture and plate thickness, causes the requirement of carbon pores liquid more and more higher.The preparation of lower concentration carbon pores liquid, can cause trouble in transport and use procedure, particularly must change tank liquor in use for some time, the tank liquor process more swapped out also can cause waste and the environmental pollution of resource.
Therefore, pcb board carbon pores liquid providing a kind of high conductivity, high density and preparation method thereof becomes extremely important.
Summary of the invention
The present invention is intended to for the deficiencies in the prior art, pcb board carbon pores liquid that a kind of high conductivity, high density are provided and preparation method thereof, the high density pcb board carbon pores solution utilizing the method to prepare metallizes, conductivity is better, it is convenient when carbon pores liquid consumes supply, tank liquor need not be changed frequently, not only safety and environmental protection but also simplify production technique, reduce the production cost of pcb board.
The present invention solves this technical problem adopted technical scheme: a kind of high density carbon pores liquid of pcb board, calculates, conductive carbon material 7-9% with the high density carbon pores liquid weight percent of the described pcb board finally completed; Tensio-active agent 4-8%; Organic dispersing agent 4-8%; Wetting agent 1-5%, pH adjusting agent, water surplus; The pH value that the amount that described pH adjusting agent uses is the high density carbon pores liquid by described pcb board is adjusted to 9.5-10.5 and is as the criterion.
Wherein, the conductive carbon material that the present invention adopts, its primary particle diameter is little, is 10-50nm, has better dispersed and higher conductivity.Primary particle diameter is that the conductive carbon material of 10-50nm can exist in the mode of reuniting; particle after reunion can be micron-sized, the effect of adding physical mechanical under the synergy of organic dispersing agent and wetting agent the grain diameter of conductive carbon material is reached 100-200 nanometer is dispersed precipitates in the solution and not.Being preferably graphitized carbon black is: the one in F900A superconductive carbon black, CabotXC-72 graphitized carbon black.F900A in F900A superconductive carbon black is the model of superconductive carbon black.It is the carbon black materials of XC-72 that CabotXC-72 graphitized carbon black refers to the type kind that Cabot Co., Ltd of the U.S. produces and sell.
Further, described tensio-active agent is one or more in polyoxyethylene alkyl ether sulfate and salt thereof.
Further, described organic dispersing agent is one or more in Sulfonates macromolecule dispersing agent.Organic dispersing agent be preferably in sodium cellulose xanghate salt, Disodium sulfosuccinate, sodium branched alkyl benzene sulfonate one or more.
Further wetting agent be preferably in JFC, PEG600, PEG1000, fast T, polyethers one or more.
Wherein, the chemical name of JFC is secondary sad polyoxyethylene acid or fatty alcohol-polyoxyethylene ether, and its chemical property is: be muddy shape when 5% aqueous solution is heated to more than 50 DEG C, reduces temperature and still can clarify.Cloud point 40 ~ 50 DEG C.Phenomenon of congealing is had during low temperature.Good stability, resistance to strong acid, alkali, hypochlorite, hard water and heavy metallic salt.Belong to nonionic surface active agent.To various fiber without avidity.The chemical name of fast T is disecoctylmaleate sodium sulfonate, for faint yellow to brown color viscous liquid.Polyethers is also known as polyglycol ether, and it is with oxyethane, propylene oxide, butylene oxide ring etc. for raw material, the simple linear polymer that open loop homopolymerization or copolymerization obtain under catalyst action.PEG600 and PEG1000, PEG refer to polyoxyethylene glycol, 600 and 1000 molecular-weight average referring to this polyoxyethylene glycol.
Further, described pH adjusting agent is sodium carbonate-bicarbonate system.
The high density carbon pores liquid and preparation method thereof of pcb board of the present invention, its step is as follows successively:
1) preparation of material A, is scattered in the wetting agent solution of described deal by the conductive carbon material of described deal, soak 12 hours, obtain described material A;
The preparation of material B, adds pH adjusting agent in the surfactant soln of described deal, after adjust ph to 9.5-10.5, adds the organic dispersing agent of described deal, stirs into clear solution, obtains described material B;
2) described material B mixes with material A, stirs, and both obtains finished product.
Wherein, described step 2) in high-speed stirring be that 1200 revs/min of ground stir.
Compared with prior art, there is following positively effect: the present invention has prepared a kind of high density carbon pores liquid of pcb board, and its conductivity is extremely strong, good stability, effective concentration are high, avoids settlement issues in use; And reduce the frequency changing tank liquor, nontoxic, pollution-free, environmentally friendly.This formula makes water-fast conductive carbon material evenly form one deck suspension by the combined action of wetting agent and organic dispersing agent, make the conductive carbon material particle diameter in suspension reach between 100-200 nanometer by the grinding of physical mechanical simultaneously, so can not sedimentation, good stability.Adjust conductive carbon material meeting uniform adsorption when producing printed circuit board (PCB) on hole wall by the electric charge of pre-treatment, after completing this operation, test resistance is had by oneself between 10-50 ohm, so conduct electricity very well.
Below in conjunction with drawings and Examples, the invention will be further described.
Accompanying drawing explanation
Fig. 1 is the DTV picture before the high density carbon pores liquid effect of pcb board of the present invention.
Fig. 2 is the DTV picture after the high density carbon pores liquid effect of pcb board of the present invention.
Fig. 3 is the DTV picture of the high Current Zone of Kazakhstan groove detection electroplating efficiency (1A electric current) of embodiment one.
Fig. 4 is the DTV picture in the low current district of Kazakhstan groove detection electroplating efficiency (1A electric current) of embodiment one.
Fig. 5 is the DTV picture of the high Current Zone of Kazakhstan groove detection electroplating efficiency (1A electric current) of embodiment two.
Fig. 6 is the DTV picture in the low current district of Kazakhstan groove detection electroplating efficiency (1A electric current) of embodiment two.
Embodiment
Embodiment one
The high density carbon pores liquid of the pcb board of the present embodiment one, calculate with the high density carbon pores liquid weight percent of the pcb board finally completed, its proportioning is:
Conductive carbon material: CabotXC-72 is 9%;
Tensio-active agent: polyoxyethylene alkyl ether sulfate is 4%;
Organic dispersing agent: sodium cellulose xanghate salt is 6%;
Wetting agent: PEG600 is 1.6%;
PH adjusting agent: sodium carbonate-bicarbonate;
Water surplus.
The step of the high density carbon pores liquid and preparation method thereof of the pcb board of preparation embodiment one is as follows:
1) material A and material B is prepared,
The preparation of material A: be scattered in by the conductive carbon material of described deal in the wetting agent solution of described deal, soaks 12 hours, obtains described material A;
The preparation of material B: add pH adjusting agent in the surfactant soln of described deal, after adjust ph to 9.5-10.5, adds the organic dispersing agent of described deal, stirs into clear solution, obtains described material B;
2) add described material A to described material B, after high-speed stirring is even, and continue stirring 2 hours, both obtain finished product.
After diluting 5 times, the performance of the high density carbon pores liquid of the pcb board of embodiment one is assessed: this carbon pores liquid can stablize a not sedimentation in month, it is hole, high Current Zone 8 that Kazakhstan groove detects electroplating efficiency (1A electric current), hole, low current district 7, this DTV sheet under the 1A electric current condition of 10 minutes all on copper, as shown in Figure 3 and Figure 4.
It should be noted that, the amount that the pH adjusting agent of the present embodiment one uses, as long as be enough to the pH value of the high density carbon pores liquid of the pcb board of the present embodiment one to be adjusted to 9.5-10.5.
Wherein, described step 2) in high-speed stirring be that 1200 revs/min of ground stir.
Embodiment two
The high density carbon pores liquid of the pcb board of the present embodiment two, calculate with the high density carbon pores liquid weight percent of the pcb board finally completed, its proportioning is:
Conductive carbon material: F900A superconductive carbon black is 7%;
Tensio-active agent: polyoxyethylene alkyl ether sulfate sodium is 8%;
Organic dispersing agent: Disodium sulfosuccinate is 4%;
Wetting agent: polyethers is 2%;
PH adjusting agent: sodium carbonate-bicarbonate;
Water surplus.
The step of the high density carbon pores liquid and preparation method thereof of the pcb board of preparation embodiment two is as follows:
1) material A and material B is prepared,
The preparation of material A: be scattered in by the conductive carbon material of described deal in the wetting agent solution of described deal, soaks 12 hours, obtains described material A;
The preparation of material B: add pH adjusting agent in the surfactant soln of described deal, after adjust ph to 9.5-10.5, adds the organic dispersing agent of described deal, stirs into clear solution, obtains described material B;
2) add described material A to described material B, after high-speed stirring is even, and continue stirring 2 hours, both obtain finished product.
After diluting 5 times, the performance of the high density carbon pores liquid of the pcb board of embodiment two is assessed: this carbon pores liquid can stablize a not sedimentation in month, it is hole, high Current Zone 8 that Kazakhstan groove detects electroplating efficiency (1A electric current), hole, low current district 7, this DTV sheet under the 1A electric current condition of 10 minutes all on copper, as shown in Figure 5 and Figure 6.
It should be noted that, the amount that the pH adjusting agent of the present embodiment two uses, as long as be enough to the pH value of the high density carbon pores liquid of the pcb board of the present embodiment two to be adjusted to 9.5-10.5.
Wherein, described step 2) in high-speed stirring be that 1200 revs/min of ground stir.
Embodiment three
The high density carbon pores liquid of the pcb board of the present embodiment three, calculate with the high density carbon pores liquid weight percent of the pcb board finally completed, its proportioning is:
Conductive carbon material: F900A superconductive carbon black is 8%;
Tensio-active agent: polyoxyethylene alkyl ether sulfate potassium is 7%;
Organic dispersing agent: sodium branched alkyl benzene sulfonate is 8%;
Wetting agent: JFC is 5%;
PH adjusting agent: sodium carbonate-bicarbonate;
Water surplus.
The step of the high density carbon pores liquid and preparation method thereof of the pcb board of preparation embodiment three is as follows:
1) material A and material B is prepared,
The preparation of material A: be scattered in by the conductive carbon material of described deal in the wetting agent solution of described deal, soaks 12 hours, obtains described material A;
The preparation of material B: add pH adjusting agent in the surfactant soln of described deal, after adjust ph to 9.5-10.5, adds the organic dispersing agent of described deal, stirs into clear solution, obtains described material B;
2) add described material A to described material B, after high-speed stirring is even, and continue stirring 2 hours, both obtain finished product.
After diluting 5 times, the performance of the high density carbon pores liquid of the pcb board of embodiment three is assessed: this carbon pores liquid can stablize a not sedimentation in month.
It should be noted that, the amount that the pH adjusting agent of the present embodiment three uses, as long as be enough to the pH value of the high density carbon pores liquid of the pcb board of the present embodiment three to be adjusted to 9.5-10.5.
Wherein, described step 2) in high-speed stirring be that 1200 revs/min of ground stir.
Compared with prior art, there is following positively effect: the present invention has prepared a kind of high density carbon pores liquid of pcb board, and its conductivity is extremely strong, good stability, effective concentration are high, avoids settlement issues in use; And reduce the frequency changing tank liquor, nontoxic, pollution-free, environmentally friendly.
The present invention is not limited to above-mentioned embodiment, if do not depart from the spirit and scope of the present invention to various change of the present invention or modification, if these are changed and modification belongs within claim of the present invention and equivalent technologies scope, then the present invention is also intended to comprise these change and modification.

Claims (8)

1. a high density carbon pores liquid for pcb board, is characterized in that: calculate with the high density carbon pores liquid weight percent of the described pcb board finally completed, conductive carbon material 7-9%; Tensio-active agent 4-8%; Organic dispersing agent 4-8%; Wetting agent 1-5%, pH adjusting agent, water surplus; The pH value that the amount that described pH adjusting agent uses is the high density carbon pores liquid by described pcb board is adjusted to 9.5-10.5 and is as the criterion.
2. the high density carbon pores liquid of pcb board as claimed in claim 1, it is characterized in that: described conductive carbon material is graphitized carbon black, its primary particle diameter is 10-50nm.
3. the high density carbon pores liquid of pcb board as claimed in claim 1, is characterized in that: described tensio-active agent is one or more in polyoxyethylene alkyl ether sulfate and salt thereof.
4. the high density carbon pores liquid of pcb board as claimed in claim 1, is characterized in that: described organic dispersing agent is macromolecule dispersing agent.
5. the high density carbon pores liquid of pcb board as claimed in claim 4, is characterized in that: described organic dispersing agent is one or more in Sulfonates macromolecule dispersing agent.
6. the high density carbon pores liquid of pcb board as claimed in claim 1, is characterized in that: described pH adjusting agent is sodium carbonate-bicarbonate system.
7. the high density carbon pores liquid of pcb board as claimed in claim 1, is characterized in that: described wetting agent is the one in JFC, fast T, polyethers.
8. the preparation method of the high density carbon pores liquid of any one pcb board described in claim 1 to 7, its step is as follows successively:
1) preparation of material A, is scattered in the wetting agent solution of described deal by the conductive carbon material of described deal, soak 12 hours, obtain described material A;
The preparation of material B, adds pH adjusting agent in the surfactant soln of described deal, after adjust ph to 9.5-10.5, adds the organic dispersing agent of described deal, stirs into clear solution, obtains described material B;
2) described material B mixes with material A, stirs, and both obtains finished product.
CN201510546799.9A 2015-08-28 2015-08-28 High-concentration carbon hole solution for PCB and preparation method thereof Pending CN105063681A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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
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
CN108834309A (en) * 2018-08-30 2018-11-16 陈伟元 A kind of graphene metallization solution and the preparation method and application thereof
CN110306198A (en) * 2019-08-05 2019-10-08 柏鸣 A kind of preparation method of nano carbon colloidal sol

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JPH09118996A (en) * 1995-08-23 1997-05-06 Mec Kk Electroplating method
CN103173824A (en) * 2013-03-01 2013-06-26 溧阳市新力机械铸造有限公司 Black hole solution for printed circuit board
CN104818506A (en) * 2015-05-28 2015-08-05 哈尔滨工业大学 Solution for metalizing printed circuit board hole

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JPH09118996A (en) * 1995-08-23 1997-05-06 Mec Kk Electroplating method
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CN104818506A (en) * 2015-05-28 2015-08-05 哈尔滨工业大学 Solution for metalizing printed circuit board hole

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
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
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
CN108834309A (en) * 2018-08-30 2018-11-16 陈伟元 A kind of graphene metallization solution and the preparation method and application thereof
CN110306198A (en) * 2019-08-05 2019-10-08 柏鸣 A kind of preparation method of nano carbon colloidal sol

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Application publication date: 20151118