A chemical copper horizontal line activator and preparation method thereof

By optimizing the formulation of chemical copper horizontal line activator, controlling palladium concentration and introducing specific additives, the problem of insufficient stability and reaction speed of activation liquid in the prior art is solved, and the backlighting ability and activation efficiency of the material after electroless copper plating are significantly improved.

CN119753649APending Publication Date: 2025-04-04NANTONG MACDERLUN MATERIAL LTD
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Patent Information

Application Number
CN202411957886.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-30
Publication Date
2025-04-04

AI Technical Summary

Technical Problem

In the existing through-hole electroless plating process, the stability and activation reaction speed of the activation liquid cannot meet the actual processing needs, and the backlighting capacity of the material after electroless copper plating is insufficient.

Method used

By optimizing the formulation system of chemical copper horizontal line activator, the palladium concentration is controlled to be 0.4-0.7 g/L, combined with the introduction of boric acid, aminopyridine, methanolpyridine and polyethylene glycol and pH control, a chemical copper horizontal line activator with good stability is prepared.

Benefits of technology

The activation time has been reduced, and the backlighting capacity of the material after electroless copper plating has been increased from level 7 to level 9, improving the activation efficiency and effect.

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Abstract

The invention relates to the technical field of activators, in particular to a chemical copper horizontal line activator and a preparation method thereof. The activator comprises at least the following substances by mass concentration: 0.4-0.8 g / L of palladium sulfate, 0.4-0.8 g / L of weak acid, 0.9-2.3 g / L of pyridine, 1.4-2.4 g / L of polyethylene glycol, and 6-14 g / L of pH regulator. By optimizing the product formula system, palladium concentration production is achieved, activation time is reduced, and material quality after chemical copper plating, especially backlight capability, is improved from original level 7 to level 9.
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Description

Technical Field

[0001] The invention relates to the technical field of activators, in particular to a chemical copper horizontal line activator and a preparation method thereof. Background Art

[0002] With the development of thin and light electronic products, printed circuit boards are also developing towards multi-layer, thin, high-order blind buried holes and filled holes, which puts forward higher requirements for chemical plating of through holes. The processing technology of chemical plating of through holes includes horizontal lines and vertical lines, but the stability of the activation solution and the activation reaction speed cannot meet the actual processing technology requirements. A Chinese patent (authorization announcement number is CN 107529563 B) discloses a chemical copper activator and a preparation method, which improves stability and reduces activation processing time by optimizing the formula system, but the material quality after chemical copper plating, especially the backlight capability, needs to be further improved. Summary of the invention

[0003] In order to solve the above problems, the present invention provides a chemical copper horizontal line activator, which realizes palladium concentration production by optimizing the product formula system, reduces the activation time, and improves the material quality after chemical copper plating, especially the backlight capability, from the original level 7 to level 9.

[0004] On one hand, the present invention provides a chemical copper horizontal line activator, which comprises at least the following substances by mass concentration: 0.4-0.8 g / L of palladium sulfate, 0.4-0.8 g / L of weak acid, 0.9-2.3 g / L of pyridine, 1.4-2.4 g / L of polyethylene glycol, 6-14 g / L of pH regulator, and the solvent is water.

[0005] As a preferred technical solution, the mass concentration of palladium sulfate is 0.4-0.7 g / L.

[0006] As a preferred technical solution, the mass concentration of the weak acid is 0.4-0.7 g / L.

[0007] As a preferred technical solution, the weak acid at least includes boric acid.

[0008] Preferably, the weak acid further comprises at least one of formic acid, acetic acid, malic acid, citric acid and oxalic acid.

[0009] Preferably, the weak acid is boric acid.

[0010] As a preferred technical solution, the mass concentration of the pyridine is 1.2-1.9 g / L.

[0011] As a preferred technical solution, the pyridines include at least aminopyridine and methanol pyridine.

[0012] Preferably, the mass ratio of aminopyridine to methanol pyridine is (0.4-0.7):(0.8-1.2).

[0013] As a preferred technical solution, the mass concentration of the polyethylene glycol is 1.8-2.2 g / L.

[0014] As a preferred technical solution, the polyethylene glycol is selected from at least one of polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600, and polyethylene glycol 800, preferably polyethylene glycol 600.

[0015] As a preferred technical solution, the mass concentration of the pH regulator is 8-11 g / L.

[0016] Preferably, the pH regulator is selected from one of liquid caustic soda, aqueous ammonia, and aqueous potassium hydroxide solution, preferably liquid caustic soda.

[0017] Preferably, the mass concentration of sodium hydroxide in the liquid caustic soda is 20-40%, preferably 32%.

[0018] The chemical copper horizontal line activator provided by the present invention ensures product stability by controlling the mass concentration of palladium in the system to be 0.4-0.7 g / L of palladium, and coordinating the introduction of boric acid, aminopyridine, methanol pyridine and polyethylene glycol and pH control, and can be continuously produced under the condition of vigorous stirring of the horizontal line, while greatly reducing the activation treatment time. In particular, the mass concentrations of boric acid, aminopyridine, methanol pyridine, polyethylene glycol and pH regulator in the control system are within a suitable range, and activation for 25 seconds under the condition of an activation temperature of 50° C. can ensure that the backlight level of the copper clad plate after chemical copper plating is level 9, greatly improving the activation efficiency while improving the activation effect.

[0019] On the other hand, the present invention provides a method for preparing a chemical copper horizontal line activator, which comprises at least the following steps: mixing water, palladium sulfate, weak acid, pyridine and polyethylene glycol and cooling the mixture, and adding a pH regulator to adjust the pH to obtain the chemical copper horizontal line activator.

[0020] As a preferred technical solution, the stirring and mixing is carried out at a temperature of 35-45°C and for a time of 1-3 hours.

[0021] Preferably, the stirring and mixing is carried out at a temperature of 40° C. and for a time of 2 hours.

[0022] As a preferred technical solution, the pH of the chemical copper horizontal line activator is 8-9, preferably 8.5.

[0023] The third aspect of the present invention provides an application of a chemical copper horizontal line activator for activating copper clad laminates.

[0024] The chemical copper horizontal line activator provided by the invention has good stability, a simple preparation method, is convenient to use, and is easy to realize large-scale industrial production and popularize and apply.

[0025] Beneficial Effects

[0026] 1. The present invention provides a chemical copper horizontal line activator, which realizes palladium concentration production by optimizing the product formula system, reduces the activation time, and improves the material quality after chemical copper plating, especially the backlight capability, from the original level 7 to level 9.

[0027] 2. The chemical copper horizontal line activator provided by the present invention ensures product stability by controlling the mass concentration of palladium in the system to 0.4-0.7 g / L of palladium, and combines the introduction of boric acid, aminopyridine, methanol pyridine and polyethylene glycol and pH control. It can be continuously produced under vigorous stirring conditions on the horizontal line, while greatly reducing the activation treatment time.

[0028] 3. The mass concentrations of boric acid, aminopyridine, methanol pyridine, polyethylene glycol and pH regulator in the control system of the present invention are within an appropriate range. Activation for 25 seconds at an activation temperature of 50°C can ensure that the backlight level of the copper-clad laminate after chemical copper plating is level 9, which greatly improves the activation efficiency and the activation effect.

[0029] 4. The chemical copper horizontal line activator provided by the present invention has good stability, a simple preparation method, is easy to use, and is easy to realize large-scale industrial production and popularize and apply. DETAILED DESCRIPTION

[0030] Examples 1-3, Comparative Examples 1-2

[0031] Examples 1-3 and Comparative Examples 1-2 of the present invention provide a chemical copper horizontal line activator, and the formula is shown in Table 1 in terms of mass concentration.

[0032] Table 1

[0033]

[0034] On the other hand, Examples 1-3 of the present invention provide a method for preparing a chemical copper horizontal line activator, comprising the following steps: stirring and mixing water, palladium sulfate, weak acid, pyridine, and polyethylene glycol, cooling the mixture to 25° C., and adding a pH adjuster to adjust the pH to obtain a chemical copper horizontal line activator.

[0035] The stirring and mixing was performed at a temperature of 40° C. and for 2 hours.

[0036] The pH of the chemical copper level activator is 8.5.

[0037] Comparative Example 1 of the present invention provides a method for preparing a chemical copper horizontal line activator. The specific implementation method is the same as that of Example 1, except that the pH value of the chemical copper horizontal line activator is 7.5.

[0038] Comparative Example 2 of the present invention provides a method for preparing a chemical copper horizontal line activator. The specific implementation method is the same as that of Example 1, except that the pH value of the chemical copper horizontal line activator is 9.5.

[0039] Performance Testing

[0040] The copper-clad laminate with holes (10 cm×10 cm) was treated with the chemical copper horizontal line activator provided in the embodiment and the comparative example, the activation temperature was 50° C., the activation time was 25 s, and the copper-clad laminate after chemical copper plating was subjected to a backlight test. The backlight level is shown in Table 2.

[0041] Table 2

[0042] Example Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Backlight level 9 9 9 7 7

Claims

1. A chemical copper horizontal line activator, characterized in that: Calculated by mass concentration, it includes at least the following substances: palladium sulfate 0.4-0.8 g / L, weak acid 0.4-0.8 g / L, pyridine 0.9-2.3 g / L, polyethylene glycol 1.4-2.4 g / L, pH adjuster 6-14 g / L, and the solvent is water.

2. The chemical copper horizontal line activator according to claim 1, characterized in that: The weak acid includes at least boric acid.

3. The chemical copper horizontal line activator according to claim 1, characterized in that: The pyridines include at least aminopyridine and methanol pyridine.

4. The chemical copper horizontal line activator according to claim 3, characterized in that: The mass ratio of the aminopyridine to methanol pyridine is (0.4-0.7):(0.8-1.2).

5. The chemical copper horizontal line activator according to claim 1, characterized in that: The polyethylene glycol is selected from at least one of polyethylene glycol 200, polyethylene glycol 400, polyethylene glycol 600 and polyethylene glycol 800.

6. The chemical copper horizontal line activator according to claim 1, characterized in that: The pH regulator is selected from one of liquid alkali, ammonia water and potassium hydroxide aqueous solution.

7. The chemical copper horizontal line activator according to claim 1, characterized in that: The mass concentration of the pH regulator is 8-11 g / L.

8. A method for preparing a chemical copper horizontal line activator according to any one of claims 1 to 7, characterized in that: The method comprises at least the following steps: mixing water, palladium sulfate, weak acid, pyridine and polyethylene glycol and cooling the mixture; adding a pH regulator to adjust the pH to obtain a chemical copper horizontal line activator.

9. The method for preparing the chemical copper horizontal line activator according to claim 8, characterized in that: The stirring and mixing is performed at a temperature of 35-45° C. and for a time of 1-3 h.

10. The method for preparing the chemical copper horizontal line activator according to claim 8, characterized in that: The pH of the chemical copper level activator is 8-9.

Citation Information

Patent Citations

  • A chemical copper activator and its preparation method

    CN107529563B