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Metal-coated polyimide resin substrate with excellent thermal aging resistance properties

A technology for coating polyimide resin and polyimide resin, which is applied in liquid chemical plating, superimposed layer plating, metal layered products, etc., can solve problems such as differences in peel strength test results, and achieve excellent effect, the effect of improving adhesion

Inactive Publication Date: 2012-01-25
JX NIPPON MINING & METALS CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] However, in the actual surface modification of polyimide resin films, substances having various molecular structures including functional groups contributing to adhesion are produced depending on the treatment conditions, so the above-mentioned methods are only limited to specific methods. The surface modified layer dyed with silver nitrate was evaluated. Even if the thickness of the modified layer in the above evaluation is the same, there is a problem that there is a difference from the actual peel strength test results.

Method used

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  • Metal-coated polyimide resin substrate with excellent thermal aging resistance properties
  • Metal-coated polyimide resin substrate with excellent thermal aging resistance properties
  • Metal-coated polyimide resin substrate with excellent thermal aging resistance properties

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047]Capton 150EN of DuPont was used as the polyimide resin film. As a surface modification method, this polyimide resin film was immersed in an aqueous potassium hydroxide solution, and washed with pure water. Then, as a catalyst application process, it is dipped in a solution obtained by mixing or reacting a silane coupling agent having a functional group having a metal-capturing ability and a noble metal compound in advance, and washed with pure water.

[0048] After this treatment, as an electroless plating process, a nickel layer of 0.15 μm is formed using an electroless nickel-boron-based plating solution, washed with pure water, and then heat-treated at 150°C to form a nickel layer of 0.05 μm and then washed with pure water. A nickel layer of 0.20 μm was formed in total. Next, an electroless copper seed layer was formed on the nickel layer in an electroless copper plating solution, and then an 8 μm copper conductor layer was formed by electroplating.

[0049] The thu...

Embodiment 2

[0056] Capton 150EN of DuPont was used as the polyimide resin film. As a surface modification method, after irradiating this polyimide resin film with UV, it immersed in sulfuric acid, and washed with pure water after that. Then, as a catalyst application process, it is dipped in a solution obtained by mixing or reacting a silane coupling agent having a functional group having a metal-capturing ability and a noble metal compound in advance, and washed with pure water.

[0057] After this treatment, as an electroless plating step, a nickel layer of 0.2 μm was formed using an electroless nickel-boron-based plating solution, followed by washing with pure water. Next, an electroless copper seed layer was formed on the nickel layer in an electroless copper plating solution, and then an 8 μm copper conductor layer was formed by electroplating.

[0058] The thus-formed metal-clad polyimide resin substrate was measured for 90° peel strength, and the polyimide thickness of the peeled ...

Embodiment 3

[0063] Capton 150EN of DuPont was used as the polyimide resin film. As a surface modification method, after irradiating this polyimide resin film with UV, it was dipped in nitric acid and washed with pure water. Then, as a catalyst application process, it is dipped in a solution obtained by mixing or reacting a silane coupling agent having a functional group having a metal-capturing ability and a noble metal compound in advance, and washed with pure water.

[0064] After this treatment, as an electroless plating process, a nickel layer of 0.15 μm is formed using an electroless nickel-boron-based plating solution, washed with pure water, and then heat-treated at 150°C to form a nickel layer of 0.05 μm and then washed with pure water. A nickel layer of 0.20 μm was formed in total. Next, an electroless copper seed layer was formed on the nickel layer in an electroless copper plating solution, and then an 8 μm copper conductor layer was formed by electroplating.

[0065] The thu...

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Abstract

Provided is a metal-coated polyimide resin substrate that exhibits a high level of adhesion after aging at 150 DEG C for 168 hours without a reduction in the initial close adhesion between a metal-coated polyimide resin film and a metal layer. The metal-coated polyimide resin substrate is produced as follows. After surface modification is applied to one surface or both surfaces of a polyimide resin film using a wet method, a dry method, or a combination thereof, a barrier layer is formed using a wet method, a seed layer is subsequently formed using a wet method or a dry method, and a conductive film is formed on the surface layer using a wet method. The metal-coated polyimide resin substrate is characterized in that the thickness of a mixed layer of a polyamide residue and a barrier-metal layer residue at the peeled surface on the conductive film layer side of said metal-coated polyimide resin substrate after the metal-coated polyimide resin substrate is subjected to a 90 DEG peel test is 2.6 nm or less, in terms of Si sputtering speed, when measured by means of a depth profile analysis using a time-of-flight secondary ion mass spectrometer (TOF-SIMS), and the peel strength retention rate after a 168-hour aging test at 150 DEG C (peel strength after aging at 150 DEG C for 168 hours / initial peel strength) is 50% or higher.

Description

technical field [0001] The present invention relates to a method for producing an adhesive-free flexible laminate that can be used as a mounting material for electronic components such as flexible printed boards, TABs, and COFs, especially a metal-clad polyimide resin substrate with excellent heat aging resistance. Background technique [0002] FCCL (Flexible Copper Clad Laminate) in which a metal conductor layer mainly composed of copper is laminated on a polyimide film is widely used as a material for circuit boards in the electronics industry. Among them, an adhesive-free flexible laminate (particularly a two-layer flexible laminate) that does not have an adhesive layer between a polyimide film and a metal layer has attracted attention as circuit wiring widths have become finer pitches. [0003] A method for producing an adhesive-free flexible laminate, especially an adhesive-free flexible laminate corresponding to a fine pitch, includes a method in which a polyimide resi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C28/02B32B15/088C23C18/20C25D5/56H05K3/24H05K3/38
CPCH05K2201/2063H05K1/0346H05K3/388C25D5/56C23C18/204H05K3/381H05K3/181H05K2201/0344H05K2201/0154C23C18/24C23C18/1651C23C18/2006Y10T428/12535Y10T428/31721B32B15/088C23C18/20C23C28/02H05K3/24
Inventor 吉田拓
Owner JX NIPPON MINING & METALS CORP
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