CN105779980B - A kind of electroless copper agent and preparation method thereof - Google Patents

A kind of electroless copper agent and preparation method thereof Download PDF

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Publication number
CN105779980B
CN105779980B CN201610131545.5A CN201610131545A CN105779980B CN 105779980 B CN105779980 B CN 105779980B CN 201610131545 A CN201610131545 A CN 201610131545A CN 105779980 B CN105779980 B CN 105779980B
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stirring
added
electroless copper
proportioning
agent
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CN105779980A (en
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***
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Jiangsu Essen semiconductor materials Limited by Share Ltd
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ASEM (SUZHOU) ELECTRONIC MATERIAL Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/38—Coating with copper
    • C23C18/40—Coating with copper using reducing agents
    • C23C18/405—Formaldehyde

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemically Coating (AREA)
  • Manufacturing Of Printed Wiring (AREA)

Abstract

The invention belongs to circuit board production techniques field, is related to a kind of electroless copper agent and preparation method thereof, wherein the component of electroless copper agent and percentage by weight are：EDTA 2Na0.03 0.04%, copper sulphate 0.005 0.007%, sodium hydroxide 0.003 0.007%, EDTP 0.002 0.005%, formaldehyde 0.002 0.004%, methanol 0.003 0.005%, adipic acid 0.01 0.05%, succinic acid 0.005 0.01%, remaining is deionized water.Electroless copper agent of the present invention can not only reach RoHS standards, and relative to CuCl2System copper plating agent adhesive force and wet-hot aging performance are stronger.

Description

A kind of electroless copper agent and preparation method thereof
Technical field
The present invention relates to circuit board production techniques field, more particularly to a kind of coating is nontoxic and coating performance is good chemical plating Copper agent and preparation method thereof.
Background technology
3D-MID is English " abbreviation of Three-dimensional Molded Interconnect Device ", Chinese Literal translate as three dimensional mold interconnecting device, be primarily referred to as making three with electric function on the plastic casing surface of injection molding Circuit is tieed up, belongs to a kind of electroless copper technology.3D-MID technologies have many kinds, include LDS (laser direct structuring technique), LRP (laser reconstruct printing) etc., wherein LDS technologies have been widely used in communication, automotive electronics, electromechanical equipment, doctor at present Treat the application fields such as apparatus.
LDS circuits copper metallization currently used in the market, more with CuCl2Based on system；Stabilizer is more with the CN that dissociates-For Main (free CN-Have severe toxicity), do not meet Europe《The instruction of some harmful components is used in electronic and electrical equipment on being limited in》 The requirement of (abbreviation RoHS).And contain substantial amounts of Cl in liquid medicine-Reducing agent formaldehyde can be made largely to volatilize in production, to employee Body damages；Also difficulty is caused to wastewater treatment.
Therefore, it is necessary to a kind of preferably scheme is provided to solve the above problems.
The content of the invention
It is a primary object of the present invention to provide the electroless copper agent and its preparation that a kind of coating is nontoxic and coating performance is good Method.
The present invention is achieved through the following technical solutions above-mentioned purpose：A kind of electroless copper agent, by EDTA-2Na, copper sulphate, Sodium hydroxide, EDTP, formaldehyde, methanol, adipic acid, succinic acid and deionized water composition, its each component content are：EDTA- 2Na0.03-0.04%, copper sulphate 0.005-0.007%, sodium hydroxide 0.003-0.007%, EDTP 0.002-0.005%, Formaldehyde 0.002-0.004%, methanol 0.003-0.005%, adipic acid 0.01-0.05%, succinic acid 0.005-0.01%, remaining For deionized water.
A kind of preparation method of electroless copper agent, includes the following steps：
1. 30% deionized water is added in a reservoir；
2. in the case of stirring, EDTA-2Na is added by proportioning, is stirred 25-30 minutes；
3. in the case of stirring, copper sulphate is added by proportioning, continues stirring 25-30 minutes；
4. in the case of stirring, sodium hydroxide is added by proportioning, continues stirring 25-30 minutes；
5. in the case of stirring, EDTP is added by proportioning, continues stirring 25-30 minutes；
6. in the case of stirring, formaldehyde, methanol, adipic acid and succinic acid are added by proportioning, continues stirring 25-30 minutes；
7. moisturizing to aequum, after the completion of stir evenly.
Using above-mentioned technical proposal, the beneficial effect of technical solution of the present invention is：Electroless copper agent of the present invention can not only reach To RoHS standards, and relative to CuCl2System copper plating agent adhesive force and wet-hot aging performance are stronger.
Embodiment
The present invention is described in further detail with reference to specific embodiment.
Embodiment 1
1. 30% deionized water is added in a reservoir；
2. in the case of stirring, 0.04%EDTA-2Na (disodium ethylene diamine tetraacetate), 25-30 points of stirring are added by proportioning Clock；
3. in the case of stirring, 0.007% copper sulphate is added by proportioning, continues stirring 25-30 minutes；
4. in the case of stirring, 0.007% sodium hydroxide is added by proportioning, continues stirring 25-30 minutes；
5. in the case of stirring, 0.005%EDTP (tetrahydroxypropyl ethylenediamine) is added by proportioning, continue to stir 25-30 points Clock；
6. in the case of stirring, 0.004% formaldehyde, 0.005% methanol, 0.05% adipic acid and 0.01% are added by proportioning Succinic acid, continues stirring 25-30 minutes；
7. moisturizing to aequum, after the completion of stir evenly.
Embodiment 2-5
The method that EXPERIMENTAL EXAMPLE 1 is repeated by each component content specified in table 1, obtains the electroless copper agent of different ratio (omitting deionized water), the agent of gained electroless copper require to test according to RoHS.
Table 1：
It will treat that plated product integrally immerses 30min, taking-up drying among electroless copper agent made from embodiment 1-5, and use CuCl2System copper plating agent is tested as reference examples.
Detection method is：
1. adhesive force is tested：Hundred lattice 3M tensile tests are repeated 3 times, and whether observation coating, which has, comes off；
2. double 85 tests：Placed in the environment of 85 DEG C of temperature, humidity 85%, when observation coating changes.
Table 2：
Adhesive force is tested Double 85 tests
Embodiment 1 Do not fall off 168 is unchanged when small
Embodiment 2 Do not fall off 168 is unchanged when small
Embodiment 3 Do not fall off 168 is unchanged when small
Embodiment 4 Do not fall off 168 is unchanged when small
Embodiment 5 Do not fall off 168 is unchanged when small
Reference examples Come off 72 interior appearance discolorations when small, aoxidize and come off
As shown in Table 2, compared to CuCl2System copper plating agent, electroless copper agent strong adhesive force of the present invention, and have well Wet-hot aging performance.
Above-described is only some embodiments of the present invention.For those of ordinary skill in the art, not On the premise of departing from the invention design, various modifications and improvements can be made, these belong to the protection model of the present invention Enclose.

Claims (2)

  1. A kind of 1. electroless copper agent, it is characterised in that：By EDTA-2Na, copper sulphate, sodium hydroxide, EDTP, formaldehyde, methanol, oneself Diacid, succinic acid and deionized water composition, its each component content are：EDTA-2Na0.03-0.04%, copper sulphate 0.005- 0.007%th, sodium hydroxide 0.003-0.007%, EDTP0.002-0.005%, formaldehyde 0.002-0.004%, methanol 0.003- 0.005%th, adipic acid 0.01-0.05%, succinic acid 0.005-0.01%, remaining is deionized water.
  2. 2. the preparation method of the electroless copper agent described in a kind of claim 1, it is characterised in that comprise the following steps：
    1. 30% deionized water is added in a reservoir；
    2. in the case of stirring, EDTA-2Na is added by proportioning, is stirred 25-30 minutes；
    3. in the case of stirring, copper sulphate is added by proportioning, continues stirring 25-30 minutes；
    4. in the case of stirring, sodium hydroxide is added by proportioning, continues stirring 25-30 minutes；
    5. in the case of stirring, EDTP is added by proportioning, continues stirring 25-30 minutes；
    6. in the case of stirring, formaldehyde, methanol, adipic acid and succinic acid are added by proportioning, continues stirring 25-30 minutes；
    7. moisturizing to aequum, after the completion of stir evenly.
CN201610131545.5A 2016-03-09 2016-03-09 A kind of electroless copper agent and preparation method thereof Active CN105779980B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610131545.5A CN105779980B (en) 2016-03-09 2016-03-09 A kind of electroless copper agent and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610131545.5A CN105779980B (en) 2016-03-09 2016-03-09 A kind of electroless copper agent and preparation method thereof

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CN105779980A CN105779980A (en) 2016-07-20
CN105779980B true CN105779980B (en) 2018-04-20

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101802264A (en) * 2007-09-05 2010-08-11 荷兰应用自然科学研究组织Tno An electroless process for depositing a metal on a non-catalytic substrate
CN103132061A (en) * 2011-11-25 2013-06-05 青州市龙宇化工科技有限公司 Electroless copper plating solution and preparation method therdof
CN105296976A (en) * 2015-10-21 2016-02-03 深圳市发斯特精密技术有限公司 Chemical-copper solution and chemical copper plating method

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5255015B2 (en) * 2010-04-28 2013-08-07 名古屋メッキ工業株式会社 Electroless copper plating method for polymer fiber

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101802264A (en) * 2007-09-05 2010-08-11 荷兰应用自然科学研究组织Tno An electroless process for depositing a metal on a non-catalytic substrate
CN103132061A (en) * 2011-11-25 2013-06-05 青州市龙宇化工科技有限公司 Electroless copper plating solution and preparation method therdof
CN105296976A (en) * 2015-10-21 2016-02-03 深圳市发斯特精密技术有限公司 Chemical-copper solution and chemical copper plating method

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Address after: 215000 1647 Huangpu Road, Qian Deng Town, Kunshan City, Suzhou, Jiangsu

Patentee after: Jiangsu Essen semiconductor materials Limited by Share Ltd

Address before: 215000 1647 Huangpu Road, Qian Deng Town, Kunshan City, Suzhou, Jiangsu

Patentee before: ASEM (Suzhou) Electronic Material Co., Ltd.