CN109082651B - Pretreatment composition for chemical plating - Google Patents
Pretreatment composition for chemical plating Download PDFInfo
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- CN109082651B CN109082651B CN201810994998.XA CN201810994998A CN109082651B CN 109082651 B CN109082651 B CN 109082651B CN 201810994998 A CN201810994998 A CN 201810994998A CN 109082651 B CN109082651 B CN 109082651B
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- acid
- pretreatment composition
- electroless plating
- plating
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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
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1841—Multistep pretreatment with use of metal first
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/10—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern
- H05K3/18—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material
- H05K3/181—Apparatus or processes for manufacturing printed circuits in which conductive material is applied to the insulating support in such a manner as to form the desired conductive pattern using precipitation techniques to apply the conductive material by electroless plating
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- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing Of Printed Wiring (AREA)
- Chemically Coating (AREA)
Abstract
The invention discloses a pretreatment composition for chemical plating, which comprises the following components: an acid free of halide ions, a source of halide ions and an unsaturated carboxylic acid. According to the invention, the acid without halide ions, the halide ion source and the unsaturated carboxylic acid are compounded, so that the prepared pretreatment composition for chemical plating can effectively remove palladium adsorbates and precipitates in a non-plating target area, thereby improving the phenomenon of 'diffusion plating' during chemical plating and improving the yield of fine circuit printed circuit boards.
Description
Technical Field
The invention relates to the field of printed circuit board preparation, in particular to a pretreatment composition for chemical plating.
Background
In the production process of Printed Circuit Boards (PCBs), electroless nickel gold plating and nickel palladium gold plating are two common final surface treatment methods for metal wiring on a Circuit Board. Electroless nickel-gold is formed by chemically plating a layer of nickel on the surface of copper, and then plating a layer of gold on the surface of nickel by a displacement reaction. The processing method enables the circuit board to have multiple functions of welding, contact conduction, routing, heat dissipation and the like.
The activation of the metallic copper surface on the circuit board is required prior to electroless nickel plating because the copper surface does not spontaneously drive the reduction of nickel ions to effect electroless nickel deposition. In industry, palladium activating solution is usually used to contact with circuit board, and electrons released after dissolving copper surface in trace amount are used to reduce palladium ions into metal palladium, so as to form a thin palladium layer on the copper surface as a catalytic catalyst for nickel deposition, thereby generating electroless deposition of nickel. However, this electroless nickel plating process typically results in palladium metal being deposited not only on the copper surface but also on other non-plated surfaces of the circuit board (e.g., solder resist inks, dry films, or bare circuit board substrates), resulting in subsequent nickel deposition not only on the copper lines, but also on the board surfaces in the vicinity of the copper lines, a phenomenon known as "strike-through". Slightly, the gold deposit is formed in a dot shape on the surface of the circuit board, which results in a thick copper surface in the case of severe cases, and in a bridge short between wiring and contact pads in the case of severe cases, and particularly, in a high-density circuit having a line width and a line pitch of about 75 μm or less, the short-circuit phenomenon is more likely to occur.
In order to avoid the above phenomenon, the industry generally adds a water washing step between the steps of treating the circuit board with the palladium activating solution and dissolving nickel, so as to remove the excessive palladium ions adsorbed on the non-plating surface. At present, a method for directly using purified water for cleaning is available in water washing, but the method can hydrolyze palladium ions to obtain palladium-containing precipitate which is adsorbed on a non-plating surface, and the precipitate enters a nickel dissolving step and then reacts with a reducing agent to form a palladium simple substance with catalytic activity, and the phenomenon of 'diffusion plating' is generated.
In order to enhance the cleaning effect, a treatment method using 1-5% sulfuric acid as a cleaning solution is also available, but the cleaning solution must be replaced frequently, otherwise, the cleaning effect cannot be achieved, and palladium adsorption on the non-plating surface is caused due to the suspension of accumulated palladium nuclei. For high density circuits, sulfuric acid washing does not adequately remove excess palladium ions and palladium hydroxide precipitates, and "bleed" still occurs resulting in short circuits of the circuit.
Therefore, the industry is eagerly looking for a suitable pretreatment composition for electroless plating.
Disclosure of Invention
Accordingly, an object of the present invention is to provide a pretreatment composition for electroless plating which is effective in removing palladium adsorbates and precipitates in a non-plating target region, thereby improving the "bleed plating" phenomenon occurring during electroless plating and improving the yield of fine line printed wiring boards.
The pretreatment composition for electroless plating comprises the following components: an acid free of halide ions, a source of halide ions and an unsaturated carboxylic acid.
Preferably, the pretreatment composition for electroless plating according to the present invention comprises the following components in concentrations, based on the total volume of the pretreatment composition: 1 to 100g/L of an acid not containing a halide ion, 0.01 to 10g/L of a halide ion source, and 0.001 to 10g/L of an unsaturated carboxylic acid.
Preferably, the pretreatment composition for electroless plating further comprises 0.001-100 g/L of non-reducing polysaccharide based on the total volume of the pretreatment composition. The pretreatment composition contains the non-reducing polysaccharide with the specific concentration, so that the surface tension of the pretreatment composition can be reduced, the pretreatment composition can better infiltrate the whole surface of the substrate, a metal coating on the substrate cannot be influenced, and especially, the excessive palladium in a non-plating area can be better cleaned under the condition that the width and the line distance of a copper wire are smaller.
Wherein the acid containing no halide is one or more selected from sulfuric acid, phosphoric acid, alkylsulfonic acid and sulfamic acid; the alkyl sulfonic acid is preferably methanesulfonic acid.
Wherein the halide ion source is selected from one or more of hydrochloric acid, sodium chloride, potassium chloride, ammonium chloride, hydrobromic acid, sodium bromide, potassium bromide and ammonium bromide.
Wherein the unsaturated carboxylic acid is selected from one or more than two compounds shown in the structure of formula (1) or formula (2),
the structure of formula (1) is as follows:
wherein R is1、R2And R3Each independently selected from hydrogen, C1-C4 alkyl which is unsubstituted or substituted by hydroxyl, carboxyl, phenyl which is unsubstituted or optionally substituted by one or more substituents selected from C1-C4 alkyl which is substituted by carboxyl, hydroxyl or hydroxyl, R1、R2And R3Only one of them is a group containing a benzene ring,
the structure of formula (2) is as follows:
wherein R is4Selected from hydrogen, carboxyl, phenyl which is unsubstituted or optionally substituted by one or more substituents selected from carboxyl, hydroxyl or C1-C4 alkyl substituted by hydroxyl.
Wherein the unsaturated carboxylic acid is one or more of cinnamic acid, m-hydroxy cinnamic acid, coumarin, crotonic acid, maleic acid and butynedioic acid.
Wherein the non-reducing polysaccharide is one or more selected from sucrose, trehalose and raffinose.
The invention also discloses a method for chemically plating metal or metal alloy, which comprises the following steps:
(1) providing a substrate with a copper surface;
(2) contacting the substrate with a noble metal ion-containing composition;
(3) cleaning the substrate obtained in the step (2) with the pretreatment composition for electroless plating;
(4) depositing a metal or metal alloy on the substrate obtained in step (3) using an electroless plating solution.
Wherein, the noble metal ion in the step (2) is palladium, the metal in the step (4) is selected from nickel or gold, and the metal alloy is nickel-phosphorus alloy.
The pretreatment composition can be applied to the cleaning step of chemical nickel (palladium) gold plating, and can also be applied to the chemical plating process of metals or metal alloys such as silver plating, lead plating, cobalt plating, lead-boron alloy plating, lead-phosphorus alloy plating, cobalt-boron alloy plating and the like.
Compared with the prior art, the invention has the following beneficial effects:
the invention prepares the pretreatment composition for electroless plating by compounding the acid without halide ions, the halide ion source and the unsaturated carboxylic acid, which can effectively remove palladium adsorbate and precipitate in a non-plating target area (the analysis principle is as follows: in the acid environment of the pretreatment composition, the palladium ions adsorbed in a non-plating area are combined by the unsaturated carboxylic acid and are carried away from the surface of a substrate through the synergistic effect of the halide ion source compound and the unsaturated carboxylic acid in a certain concentration range, and the palladium precipitate is dissolved to become palladium ions which are cleaned out of the surface of the substrate by the composition, thereby achieving better cleaning effect of redundant palladium, and the condition that the palladium precipitate is re-adsorbed to the surface of the substrate due to the accumulation of palladium nuclei does not occur in the cleaning step, moreover, the pretreatment composition does not corrode the palladium catalyst simple substance layer deposited on the copper surface, affecting the subsequent electroless plating step. ) Thereby improving the phenomenon of 'diffusion plating' during chemical plating and improving the yield of the fine line printed circuit board.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. The present invention may be embodied in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In the following detailed description, unless otherwise specified, all conventional methods are used; the raw materials, reagents, and the like used in the following embodiments are all commercially available products unless otherwise specified.
The substrate can be a conventional PCB (Printed Circuit board), and mainly comprises a hard board and a soft board (FPC), wherein the hard board can be made of resin, glass (glass fiber), plastic, ceramic, stone, the soft board and the like, and the soft board can be made of polyimide, polyethylene terephthalate, aramid fiber ester, polyvinyl chloride and the like.
The "unsaturated carboxylic acid" in the present invention may be commercially available or may be obtained according to a production method described in a patent, a literature, and a textbook which have been disclosed so far, for example, CN1539808A, US5250729A, US5808148A, or US 20150038735A.
The pretreatment composition for electroless plating according to the present invention can be prepared by a conventional method, that is, an acid free of halide ions, a halide ion source and an unsaturated carboxylic acid capable of obtaining a desired concentration are separately weighed and dissolved in an appropriate amount of water, and if containing a non-reducing polysaccharide, the above steps are also dissolved in water, and finally the whole solution is fixed to a fixed volume.
The general procedure for electroless nickel/gold plating on microetched copper-containing circuit substrates is as follows:
copper circuit substrate → activation → cleaning → electroless nickel plating → electroless gold plating
A water washing step can be added between every two steps.
An activation step: the activating solution can be palladium ion activating solution commonly used in the industry, and the activating solution used in the invention is the activating solution containing 30mg/L palladium ions and 50g/L sulfuric acid. While the palladium activation time for the copper surface is generally about 1 minute, the activation time of the embodiment of the present invention is extended to 5 minutes, so that more palladium ions are attached to the non-plating region of the substrate, to embody the cleaning step, the pretreatment composition for electroless plating according to the present invention has a better effect of removing excess palladium than the existing sulfuric acid cleaning solution, and the temperature of the activation step is room temperature.
A cleaning step: the pretreatment composition for electroless plating can be used for removing palladium in a non-plating area at room temperature, the preferred operating temperature range is 20-40 ℃, the operating time is generally 30-300 seconds, and the preferred time is 30-60 seconds. The cleaning temperature in the examples of the present invention was room temperature, and the cleaning time was 1 minute.
Chemical nickel plating step: the nickel bath may be an electroless nickel bath commonly used in the industry, and the bath used herein is a 5183 series nickel bath (commercially available, available from Guangdong technologies, Inc.), operating at 80 deg.C, pH 4.3, and time 20 minutes.
Chemical gold plating: the gold bath may also be an electroless gold bath commonly used in the art, and the bath used herein is a 5185 series gold bath (commercially available, available from Guangdong technologies, Inc.) operating at 82 deg.C, pH 4.4, and time 6 minutes.
EXAMPLES 1-10 preparation of pretreatment composition for electroless plating
Acid, halide ion source and unsaturated carboxylic acid and/or non-reducing polysaccharide which can obtain the expected concentration and do not contain halide ions are respectively weighed according to the following table 1, are sequentially dissolved in 1.5L of water, and finally the volume is determined to be 2L for subsequent cleaning effect tests.
Comparative example 11 sulfuric acid solution
TABLE 1
Concentration unit: g/L
Examples 12 to 21 cleaning effect test of application of pretreatment composition for electroless plating
Comparative example 22 application of sulfuric acid cleaning solution cleaning effect test
Prepared were 11 FR-4 epoxy resin/glass fiber rigid boards containing copper wiring and 11 polyimide resin FPC boards, which were subjected to conventional microetching, each having a size of 10cm × 10cm, and each having a line width and a line pitch of 75 μm on the substrate. The substrates are prepared by the steps of carrying out nickel-gold plating on the copper-containing circuit board, and depositing metal nickel and gold on the substrates through the processes of activation, cleaning, electroless nickel plating and electroless gold plating, wherein the cleaning steps are respectively carried out by using the pretreatment composition for electroless plating prepared in the above examples 1-10 and the sulfuric acid cleaning solution of the comparative example 11.
And observing the nickel-gold diffusion plating condition of the copper circuit on all the substrates subjected to nickel-gold melting under a metallographic microscope. The ratio of the line spacing after nickel and gold melting to the original line spacing is used for representing the diffusion plating condition of the copper circuit in the test, the larger the numerical value is, the smaller the line spacing change is, the more slight the diffusion plating condition is, otherwise, the diffusion plating condition is more serious.
Each pretreatment composition was cleaned from 1 hard and 1 soft board and numbered 1 and 2, respectively, for example, the composition of example 1 was used to treat substrates having hard boards numbered 1-1 and FPC boards numbered 1-2, and so on, and the results of the tests are shown in Table 2.
TABLE 2 cleaning test results of the pretreatment composition for electroless plating according to the present invention on excess palladium
And (4) analyzing results:
(1) examples 12-21 were cleaned using the pretreatment composition for electroless plating according to the present invention, and after electroless nickel-gold plating, the pitch was at least 70% (hard plate) and 79% (soft plate) of the original pitch, whereas comparative example 22 was cleaned using a sulfuric acid cleaning solution, and after electroless nickel-gold plating, the pitch was only 49% (hard plate) and 53% (soft plate) of the original pitch. Therefore, the pretreatment composition for electroless plating can effectively remove excessive palladium adsorption of a non-plating area, and can effectively prevent the phenomenon of 'diffusion plating' of bridging between a copper wire and a copper surface.
(2) The pretreatment compositions for electroless plating used in examples 12 and 13 contained the same acid containing no halide ion, a halide ion source, and an unsaturated carboxylic acid, and the concentrations of the above components were also the same, but the pretreatment composition for electroless plating of example 13 further contained a non-reducing polysaccharide (sucrose). From the cleaning test results, the cleaning effect of example 13 was better than that of example 12. The wire pitch after electroless plating of the hard sheet treated with the pretreatment composition for electroless plating of example 2 was 87% of the original wire pitch and the wire pitch of the soft sheet was 92%, whereas the wire pitch after electroless plating of the hard sheet treated with the pretreatment composition for electroless plating of example 1 was 75% of the original wire pitch and the wire pitch of the soft sheet was 82%. Similar results were also found in the cleaning effect tests of examples 14 and 15. The above results indicate that the pretreatment composition for electroless plating containing the non-reducing polysaccharide has a better cleaning effect than the composition containing no non-reducing polysaccharide.
Claims (8)
1. A pretreatment composition for electroless plating, characterized by consisting of: a halide-free acid, a source of halide ions and an unsaturated carboxylic acid;
based on the total volume of the pretreatment composition, the following concentrations of components were included: 1-100 g/L of acid without halide ions, 0.01-10 g/L of halide ion source and 0.001-10 g/L of unsaturated carboxylic acid;
the unsaturated carboxylic acid is selected from one or more than two compounds shown in the structure of formula (1) or formula (2),
the structure of formula (1) is as follows:
wherein R is1、R2And R3Each independently selected from hydrogen, C1-C4 alkyl which is unsubstituted or substituted by hydroxyl, carboxyl, phenyl which is unsubstituted or optionally substituted by one or more substituents selected from C1-C4 alkyl which is substituted by carboxyl, hydroxyl or hydroxyl, R1、R2And R3Only one of them is a group containing a benzene ring,
the structure of formula (2) is as follows:
wherein R is4Selected from hydrogen, carboxyl, phenyl which is unsubstituted or optionally substituted by one or more substituents selected from carboxyl, hydroxyl or C1-C4 alkyl substituted by hydroxyl;
the acid not containing halide is one or more selected from sulfuric acid, phosphoric acid, alkylsulfonic acid, and sulfamic acid.
2. The pretreatment composition for electroless plating according to claim 1, further comprising 0.001 to 100g/L of a non-reducing polysaccharide, based on the total volume of the pretreatment composition.
3. The pretreatment composition for electroless plating according to claim 1, wherein the halide-free acid is selected from methanesulfonic acid.
4. The pretreatment composition for electroless plating according to claim 1, wherein the halide ion source is one or more selected from the group consisting of hydrochloric acid, sodium chloride, potassium chloride, ammonium chloride, hydrobromic acid, sodium bromide, potassium bromide and ammonium bromide.
5. The pretreatment composition for electroless plating according to claim 1, wherein the unsaturated carboxylic acid is one or more selected from the group consisting of cinnamic acid, m-hydroxycinnamic acid, coumarin, crotonic acid, maleic acid, and butynedioic acid.
6. The pretreatment composition for electroless plating according to claim 2, wherein the non-reducing polysaccharide is one or more selected from sucrose, trehalose and raffinose.
7. A method of electroless plating a metal or metal alloy comprising the steps of:
(1) providing a substrate with a copper surface;
(2) contacting the substrate with a noble metal ion-containing composition;
(3) cleaning the substrate obtained in step (2) with the pretreatment composition according to any one of claims 1 to 6;
(4) depositing a metal or metal alloy on the substrate obtained in step (3) using an electroless plating solution.
8. The method of claim 7, wherein the noble metal ion in step (2) is palladium, the metal in step (4) is selected from nickel or gold, and the metal alloy is a nickel-phosphorus alloy.
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| CN113737159B (en) * | 2021-08-30 | 2024-08-20 | 广东东硕科技有限公司 | Presoaking liquid for inhibiting copper surface chemical plating and infiltration plating, and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1461584A (en) * | 2000-07-27 | 2003-12-10 | 阿托特希德国有限公司 | Improved adhesion of polymeric materials to metal surfaces |
| CN103189149A (en) * | 2010-09-13 | 2013-07-03 | 凯密特尔有限责任公司 | Method for coating surfaces and use of the articles coated using said method |
| CN106029946A (en) * | 2014-02-21 | 2016-10-12 | 安美特德国有限公司 | Pre-treatment process for electroless plating |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1461584A (en) * | 2000-07-27 | 2003-12-10 | 阿托特希德国有限公司 | Improved adhesion of polymeric materials to metal surfaces |
| CN103189149A (en) * | 2010-09-13 | 2013-07-03 | 凯密特尔有限责任公司 | Method for coating surfaces and use of the articles coated using said method |
| CN106029946A (en) * | 2014-02-21 | 2016-10-12 | 安美特德国有限公司 | Pre-treatment process for electroless plating |
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