CN115449794A - Low-microetching coarsening and microetching liquid, preparation method thereof and copper surface coarsening method - Google Patents
Low-microetching coarsening and microetching liquid, preparation method thereof and copper surface coarsening method Download PDFInfo
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- CN115449794A CN115449794A CN202211119452.2A CN202211119452A CN115449794A CN 115449794 A CN115449794 A CN 115449794A CN 202211119452 A CN202211119452 A CN 202211119452A CN 115449794 A CN115449794 A CN 115449794A
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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
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F1/00—Etching metallic material by chemical means
- C23F1/10—Etching compositions
- C23F1/14—Aqueous compositions
- C23F1/16—Acidic compositions
- C23F1/18—Acidic compositions for etching copper or alloys thereof
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- ing And Chemical Polishing (AREA)
- Manufacturing Of Printed Wiring (AREA)
Abstract
The invention discloses a low-microetching coarsening microetching liquid, a preparation method thereof and a copper surface coarsening method, belonging to the technical field of electronic chemical reagents for printed circuit boards. The low-microetching-amount roughening microetching solution is an acidic aqueous solution comprising 6.5-200g/L of divalent copper ion donor, 0.2-5g/L of halogen ion donor and 1-200g/L of organic acid, and has a very low halogen ion concentration compared with the existing roughening microetching solution, so that the solubility of monovalent copper ions formed in a system can be reduced, the monovalent copper ions are more easily precipitated on the copper surface in an insoluble form to form an uneven interface, the adhesion between the copper surface and resin can be enhanced, and the excellent adhesion between the copper surface and the resin under a low etching amount can be realized.
Description
Technical Field
The invention relates to a low-microetching-amount roughening microetching solution, a preparation method thereof and a copper surface roughening method, belonging to the technical field of electronic chemical reagents for printed circuit boards.
Background
In recent years, with the rapid development of narrow pitches of wiring, printed circuit boards need to have smaller etching amount, and at the same time, the printed circuit boards need to be capable of forming better bonding force with resin and forming better coarsening appearance under the condition of the smaller etching amount.
With the continuous miniaturization of the line width/line distance and thickness of the pattern lines, the conventional chemical roughening micro-etching solution cannot meet the use requirements. In the semi-additive process (SAP), for example, the production method of the pattern circuit is: firstly, coating a seed layer of a conductive layer on a dielectric substrate, wherein the seed layer is coated by a method comprising sputtering or chemical plating; a patterned resist layer is then formed on the seed layer and the desired circuit pattern is formed by depositing a layer of electroplated copper on the seed layer, followed by differential etching. The copper layer thickness of the deposited electroplated copper, whether electroless or sputtered, is small, generally below 0.5 μm. At present, a sulfuric acid pickling method is usually adopted for such a base copper with a small thickness, and although the pickling method can remove oxides on the surface of the copper layer, the cleaning effect of grease on the surface of the copper layer is general, and in order to improve the cleaning effect, the etching amount needs to be increased. However, in the case of the conventional roughening solutions, both of the organic acid-based roughening solutions and the inorganic acid-based roughening solutions, the etching depth is large, and the roughening results in deep unevenness, which causes problems such as high resistance and disconnection in the case of a thin copper layer. And the low micro-etching amount and super-roughening can be used for roughening the surface of the uniform and concave-convex copper layer by using a smaller etching amount, so that the binding force between the base copper such as sputtered copper, chemical copper and the like and the base materials such as a copper plating-resistant dry film and the like can be remarkably improved.
Disclosure of Invention
In order to solve the above problems, the present invention provides a roughening microetching solution having a low microetching amount, which can maintain a high adhesion between a copper layer and a resin while realizing a microetching amount on a copper surface, a method for producing the same, and a method for roughening a copper surface.
The term "copper" or "copper layer" as used herein refers to a relatively thin, bulky copper layer or copper wiring layer, such as chemical copper or sputtered copper.
The technical scheme of the invention is as follows:
the invention discloses a low-microetching coarsening microetching solution which is an acidic aqueous solution comprising a divalent copper ion donor, a halogen ion donor and an organic acid.
Divalent copper ion donor
The divalent copper ion donor mainly provides divalent copper ions for the roughening microetching solution. The divalent copper ions mainly act as an oxidant in the roughening microetching solution, and can oxidize copper atoms into monovalent or divalent copper ions. Since the halide copper salt provides a part of halide ions, and the higher concentration of the halide ions increases the solubility of monovalent copper ions, which may cause an increase in etching rate, and it is difficult to control the etching amount, the divalent copper ion donor is mainly selected from at least one of an organic copper salt, an inorganic copper salt containing no halide ions, and a copper-containing oxide. Wherein the organic acid copper salt can be selected from copper formate, copper acetate, etc., but is not limited thereto; wherein the inorganic copper salt without halogen ion can be selected from copper sulfate, copper nitrate, etc., but not limited thereto; the copper-containing oxide can be selected from copper oxide, cuprous oxide, copper hydroxide, etc., but is not limited thereto. The divalent copper ion donor provides a divalent copper ion concentration of 6.5 to 200g/L, preferably 15 to 100g/L, and more preferably 30 to 50g/L. The formation of monovalent copper ions can be effectively controlled by properly adjusting the concentration of divalent copper ions.
Halogen ion donor
The halogen ion donor mainly provides halogen ions for the roughening micro-etching solution, and the halogen ions can increase the dissolution of copper and enhance the adhesion of the surface of the copper layer. The halide ion donor may be at least one selected from the group consisting of sodium chloride, calcium chloride, copper chloride, potassium chloride, ferric chloride, sodium bromide, calcium bromide, potassium bromide, etc., but is not limited thereto. The inventor researches to find that the coarsening morphology formed by the chloride ions is more uniform, and therefore, the halide ion donor is preferably chloride. The halide ion donor provides a halide ion concentration of 0.2 to 5g/L, preferably 0.2 to 4.2g/L, more preferably 0.3 to 4.2g/L, and further preferably 0.4 to 4.2g/L. When the etching amount is controlled to be about 0.1 μm, the concentration of the halide ion is preferably 0.5g/L-3.0g/L; when the etching amount is controlled to be about 0.2 μm, the halide ion concentration is most preferably controlled to be between 1.2g/L and 3.8 g/L.
Organic acids
The organic acid mainly functions to dissolve the solid divalent copper ion donor (mainly containing copper oxide) and simultaneously serves to adjust the pH of the roughening microetch solution. The organic acid is at least one of saturated fatty acid and/or at least one of unsaturated fatty acid and/or at least one of non-fatty acid, and preferably one or two of the following organic acids are combined. Among them, saturated fatty acids may be preferably, but not limited to, formic acid, acetic acid, propionic acid, butyric acid, etc.; among them, unsaturated fatty acids may be preferably, but not limited to, acrylic acid and the like; among them, non-fatty acids may be preferably, but not limited to, malic acid, citric acid, lactic acid, benzoic acid, succinic acid, oxalic acid, sulfinic acid, sulfonic acid, pyruvic acid, aconitic acid, etc. The concentration of the organic acid is 1 to 200g/L, preferably 5 to 150g/L, and more preferably 10 to 100g/L.
Cationic amine-based polymers
In order to promote coarsening and adjust the coarsening uniformity, and adjust the coarsening structure, an appropriate amount of amine-based polymer may be added to the coarsening microetching solution, and in this application, a cationic amine-based polymer is preferably added, and more preferably, but not limited to, polyethyleneimine, a diamine-based urea polymer, and the like. The weight average molecular weight of the above cationic amine-based polymer is optimally not less than 2000 and the concentration of the amount thereof is not more than 0.01g/L, preferably not more than 0.005g/L, more preferably not more than 0.001g/L.
The roughening microetching solution can also comprise other surface additives, such as conventional additives like defoaming agents, and details are not repeated in the application.
The invention also discloses a preparation method of the coarsening micro-etching solution, which comprises the following steps: firstly, placing organic acid with the formula amount in water, uniformly stirring, then adding a divalent copper ion donor with the formula amount, uniformly stirring until the solution is clear, then adding a halogen ion donor with the formula amount and other auxiliary agents such as cationic amino polymer and other surface additives, and uniformly stirring to form the coarsening micro-etching solution.
The invention also discloses a copper surface roughening method, which comprises the following steps:
and fully contacting the coarsening micro-etching solution with the surface of the copper at the temperature of between 20 and 40 ℃ to coarsen the surface of the copper. Wherein the micro-etching solution is coarsened by contacting the copper surface in one of spraying and soaking. When the coarsening micro-etching solution contacts the copper surface in a spraying mode, the spraying temperature is 20-40 ℃, and the spraying pressure is 0.05-0.5MPa; when the roughening micro-etching solution is contacted with the copper surface by using a soaking mode, the soaking temperature is 20-40 ℃, and the soaking time is 40-80s.
And (3) washing the roughened copper surface by using an acidic aqueous solution to prevent the roughened copper surface from being oxidized after contacting with air, and then washing by using deionized water and drying. Of these, the acidic aqueous solution is preferably an aqueous solution of an inorganic acid, and in the present application, an aqueous solution of hydrochloric acid having a concentration of 5 to 6vol.% is preferred.
The beneficial technical effects of the invention are as follows:
compared with the existing roughening micro-etching liquid, the roughening micro-etching liquid provided by the invention has very low halogen ion concentration. The invention reduces the concentration of halide ions in the roughening microetching solution, thereby reducing the solubility of monovalent copper ions formed in the system (part of the monovalent copper ions are formed by reducing divalent copper ions, and the other part of the monovalent copper ions are formed by oxidizing copper atoms) in the liquid system, the undissolved monovalent copper ions are easy to precipitate on the copper surface in the form of insoluble substances, particularly the monovalent copper ions formed by oxidizing the copper atoms are easy to precipitate on the copper surface, and the insoluble substances form an uneven interface on the copper surface, thereby enhancing the adhesion between the copper surface and resin, and further realizing excellent adhesion between the copper surface and the resin under low etching amount.
Detailed Description
In order to clearly understand the technical means of the present invention and to implement the technical means according to the content of the specification, the following embodiments are further described in detail in the following, which are used for illustrating the present invention and are not used to limit the scope of the present invention.
The invention is based on the following principle: the divalent copper ions react with some substances having a certain reducibility to form a compound containing monovalent copper ions, which is hardly soluble in water. The following reactions take place as in the presence of halide ions: cu 2+ + 2X - + Cu =2CuX, wherein X - Is a halogen ion, and the formed CuX is a precipitate which is insoluble in water, such as CuCl, cuBr and the like.
The roughening microetching solution was prepared according to the following preparation method in accordance with the formulation amounts shown in the respective specific examples and comparative examples in tables 1 and 2 below: the organic acid with the formula amount is placed in water and stirred uniformly, then the divalent copper ion donor with the formula amount is placed in the water and stirred uniformly until the solution is clear, then the halide ion donor with the formula amount and other additives, such as cationic amino polymer and other surface additives (other surface additives are not listed in the specific embodiment, and can be added according to needs in actual operation) are placed in the water and stirred uniformly to form the coarsening micro-etching solution.
TABLE 1 specific examples the amounts of the components (unit: g/L)
In the following comparative examples, group a was compared with the composition of example 2 (the important point is the effect of a single halogen ion concentration on peel strength under the same etching amount), and group B was compared with the composition of example 4 (B1 and B2 are the effects of the amount of cationic amine-based polymer on peel strength, and B3 to B6 are the effects of the divalent copper ion concentration on peel strength), and the amounts of the components in each ratio are shown in table 2.
TABLE 2 comparative examples the amounts of the components (unit: g/L)
Using the roughening microetching solution prepared in each of the above specific examples and comparative examples, a performance test of adhesion of resin between a copper layer and resin was performed by the following test method:
a plated surface of a test piece having a thickness of 20 μm of electrolytic copper foil was formed thereon, and etching was performed by adjusting etching time based on etching amounts of 0.1 μm, 0.2 μm and 0.4 μm by spraying or immersing the roughening microetching solution (30 ℃) of the examples shown in the table under a spray pressure (under a condition of 0.05 MPa). Then, the etching-treated surface was subjected to acid washing and water washing, and sprayed with 5% hydrochloric acid at a temperature of 25 ℃ for 15 seconds, and then washed with water and dried. A photosensitive liquid solder resist ("SR-7300G" made by hitachi) was applied to the etched surface of each copper foil after drying in a thickness of 20 μm and cured to form a composite. After a copper-clad laminate having a thickness of 1.6mm was attached to the surface of the solder resist layer of the composite with an adhesive to form a reinforcing plate, only the copper foil portion was cut into a linear shape having a width of 1 cm. Peel strength between the copper foil cut in a linear shape and the solder resist layer.
The test results of the above-described specific examples and comparative examples are shown in the following data in Table 3:
TABLE 3 results of the Performance test of the specific examples and comparative examples
Note: x in Table 3 - Represents a halogen ion (e.g. Cl) - Or Br - ）。
As can be seen from the data shown in Table 3, in examples 1 to 10, when the components and the amounts of the components described in the present application were used, a good peel strength was achieved by controlling the concentrations of cupric ion and chloride ion at low microetching amounts (0.1 μm, 0.2 μm, 0.4 μm).
In the case of the same etching amount and the same divalent copper ion concentration, the other components and the compounding ratio were the same, and only the chloride ion concentration was different, as can be seen from example 2 and comparative examples A1 to A5, the peel strength gradually decreased as the chloride ion concentration increased. As can be seen from A1-A3, when the concentration of chloride ions is more than 4.2g/L, the peel strength is lower and is lower than 0.65N/mm; when the concentration of the chloride ions is less than 0.4g/L, although the peeling strength is enhanced compared with that of A1-A3 under the same etching amount, the peeling strength is still lower and is only between 0.72 and 0.76N/mm; on the other hand, as can be seen from examples 1 and 2 (especially example 2) of the present application, when the chloride ion concentration is preferably within the range defined by the present invention, the peel strength is the best and can be 1.1N/mm or more in combination with the divalent copper ion concentration defined by the present invention.
Under the condition of the same etching amount and the same chloride ion concentration, other components and proportions are consistent, and the divalent copper ion concentration is different, as can be seen from example 4 and comparative examples B3-B5, the peeling strength is gradually increased along with the increase of the divalent copper ion concentration; however, in combination with comparative example B6, it can be seen that when the concentration of cupric ions is more than 60g/L, the peel strength is slightly decreased from that of example 4. When the concentration of the chloride ion is within the range of the divalent copper ion defined by the invention, the optimal peeling strength can be achieved under the same etching amount.
In the present invention, the copper atoms and the divalent copper ions are chemically reacted to generate monovalent copper ions in the form of insoluble substances, and the interaction between the concentration of the chloride ions and the concentration of the divalent copper ions affects the amount of monovalent copper ions formed on the surface of copper in the form of insoluble substances, so that the excessively high or low concentration of the chloride ions and the excessively high or low concentration of the divalent copper ions affect the adhesion between the final resin and the copper surface, i.e., the peel strength.
Furthermore, considering only the effect of the cationic amine-based polymer, with the other influencing factors being the same, see example 4 and comparative examples B1-B2. Wherein B2 is the case without the use of the cationic amine-based polymer, which is only 0.49N/mm as compared with the peel strength of 0.94N/mm of example 4; wherein B1 is an amount of the cationic amine-based polymer used which is larger than the amount defined herein (not higher than 0.01 g/L), which is 0.72N/mm in peel strength, as compared with 0.94N/mm in peel strength of example 4, which is larger than the case where this component is not used, but is lower than the case where the amount is used within the range defined herein. This is because when the cationic amine-based polymer of a polymer having a relatively high molecular weight (weight average molecular weight of not less than 2000) has a relatively high content, the long chain blocks the contact between the divalent copper ion and the halogen ion with the copper surface, thereby increasing the difficulty of generating monovalent copper ions, and reduces the probability of the monovalent copper ion insoluble adhering to the copper surface, resulting in poor or uneven roughened morphology of the copper surface, and further resulting in a reduction in peel strength.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The low microetching amount roughening microetching solution is an acidic aqueous solution comprising a divalent copper ion donor, a halogen ion donor and an organic acid, wherein the divalent copper ion donor provides divalent copper ions with the concentration of 6.5-200g/L, the halogen ion donor provides halogen ions with the concentration of 0.2-5g/L, and the organic acid has the concentration of 1-200g/L.
2. The low microetching coarsening microetching liquid according to claim 1, wherein: the concentration of the divalent copper ions provided by the divalent copper ion donor is 15-100g/L.
3. The low microetching coarsening microetch solution of claim 2, wherein: the divalent copper ion donor provides divalent copper ion concentration of 30-50g/L.
4. The low microetching coarsening microetching liquid according to claim 1, wherein: the cupric ion donor is at least one of organic copper salt, inorganic copper salt without halogen ion and copper-containing oxide.
5. The low microetching coarsening microetching liquid according to claim 1, wherein: the halide ion donor provides a halide ion concentration of 0.4 to 4.2g/L.
6. The low microetching coarsening microetching liquid according to claim 1, wherein: the halide ion donor is chloride.
7. The low microetching coarsening microetching liquid according to claim 1, wherein: the organic acid is at least one of saturated fatty acid and/or at least one of unsaturated fatty acid and/or at least one of non-fatty acid.
8. The low microetching coarsening microetch solution of claim 1, wherein: also comprises a cationic amine-based polymer with the concentration not higher than 0.01g/L, and the weight average molecular weight of the cationic amine-based polymer is not lower than 2000.
9. A method for preparing a low microetching roughening microetching solution according to any one of claims 1 to 8, wherein: firstly, placing organic acid with the formula amount in water, uniformly stirring, then adding a divalent copper ion donor with the formula amount, uniformly stirring until the solution is clear, then adding a halogen ion donor with the formula amount and other auxiliary agents, and uniformly stirring to form the coarsening micro-etching solution.
10. A method for roughening a copper surface, comprising:
fully contacting the copper surface with a low microetching amount roughening microetching solution according to any one of claims 1 to 8 at 20-40 ℃; and (4) washing the roughened copper surface by using an inorganic acid aqueous solution, washing by using deionized water, and drying.
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| CN111094628A (en) * | 2017-09-22 | 2020-05-01 | Mec股份有限公司 | Copper microetching agent, method for roughening copper surface, and method for producing wiring board |
| CN114672807A (en) * | 2022-05-26 | 2022-06-28 | 深圳市板明科技股份有限公司 | Organic acid super-roughening micro-etching solution with high copper content and application thereof |
| CN114959706A (en) * | 2022-07-27 | 2022-08-30 | 昆山市板明电子科技有限公司 | Organic acid type coarsening micro-etching liquid and preparation method thereof |
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2022
- 2022-09-15 CN CN202211119452.2A patent/CN115449794A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20140326696A1 (en) * | 2012-09-28 | 2014-11-06 | Mec Company Ltd. | Microetching solution for copper, replenishment solution therefor and method for production of wiring board |
| CN111094628A (en) * | 2017-09-22 | 2020-05-01 | Mec股份有限公司 | Copper microetching agent, method for roughening copper surface, and method for producing wiring board |
| CN111020584A (en) * | 2019-12-23 | 2020-04-17 | 昆山市板明电子科技有限公司 | Copper surface micro-etching roughening solution and preparation method thereof |
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