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Palladium plating liquid for preparing Co/Pd nano-multilayer film by double-flute method electrocrystallization

A nano-multi-layer and electro-crystallization technology, which is applied in the application of magnetic film to substrate, circuits, electrical components, etc., can solve the problems that Co/Pd nano-multi-layer film is easy to break and fall off, and the magnetic properties are greatly affected.

Inactive Publication Date: 2009-04-08
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Owing to finding that general Pd bath is not suitable for electrocrystallization to prepare Co / Pd nano-multilayer film in the preparation of Co / Pd nanometer multilayer film by double tank method electrocrystallization, especially the thin film obtained by palladium plating solution has high stress, makes preparation The Co / Pd nano-multilayer film is easy to break and fall off, which has a great influence on its magnetic properties

Method used

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  • Palladium plating liquid for preparing Co/Pd nano-multilayer film by double-flute method electrocrystallization
  • Palladium plating liquid for preparing Co/Pd nano-multilayer film by double-flute method electrocrystallization
  • Palladium plating liquid for preparing Co/Pd nano-multilayer film by double-flute method electrocrystallization

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Experimental program
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Effect test

Embodiment 1

[0019] Plating solution composition:

[0020] Dichlorodiamine palladium 3g / L (calculated as Pd)

[0021] Cerium sulfate 0.02g / L (calculated as Ce)

[0022] Ethylenediamine 65mL / L

[0023] Pyridine-3-sulfonic acid 0.05g / L

[0024] Sodium sulfate 30g / L

[0025] The plating solution was adjusted to pH=8.5 with ammonia water and hydrochloric acid, and the working electrode was single crystal Si(111) (with HF and HNO at a volume ratio of 3:1 3 Mixed acid etching→washing→air drying), the temperature of the plating solution is 25°C, the time for multilayer palladium plating is 30s, and the time for cobalt plating is 2s. Ammonia exposure testing (24 hours at room temperature) was performed and no breakage and cracking of the multilayer film was observed. figure 2 It is the surface topography diagram of the palladium plating, and the palladium plating layer is dense and uniform.

Embodiment 2

[0027] Plating solution composition:

[0028] Dichlorodiamine palladium 3g / L (calculated as Pd)

[0029] Cerium nitrate 0.02g / L (calculated as Ce)

[0030] Ethylenediamine 70mL / L

[0031] Ammonium pyridine-3-sulfonate 0.05g / L

[0032] Sodium sulfate 30g / L

[0033] The plating solution was adjusted to pH=9.0 with ammonia water and hydrochloric acid, and the working electrode was single crystal Si(111) (with HF and HNO at a volume ratio of 3:1 3 Mixed acid etching→washing→air drying), the temperature of the plating solution is 25°C, the time for multilayer palladium plating is 30s, and the time for cobalt plating is 2s. Ammonia exposure test (24 hours at room temperature), no cracks and cracks were observed in the multilayer film. And the magnetic properties of the Co / Pd multilayer film were tested. The hysteresis loop squareness of the Co / Pd metal nano-multilayer film Better, its coercive force can reach 1130 Oe. image 3 shown.

Embodiment 3

[0035] Bath composition

[0036] Dichlorodiamine palladium 3g / L (calculated as Pd)

[0037] Cerium sulfate 0.02g / L (calculated as Ce)

[0038] Ethylenediamine 65mL / L

[0039] Ammonium pyridine-3-sulfonate 0.06g / L

[0040] Sodium sulfate 30g / L

[0041] The plating solution was adjusted to pH=8.5 with ammonia water and hydrochloric acid, and the working electrode was single crystal Si(111) (with HF and HNO at a volume ratio of 3:1 3 Mixed acid etching→washing→air drying), the temperature of the plating solution is 25°C, and the deposition time of multilayer coating Co and Pd is extended to 120s and 600s, respectively. As a result, the layered structure of the Co layer and the Pd layer is clear and continuous. The thickness of the layer is about 120nm and it is shiny. The ammonia exposure test (24 hours at room temperature) of the coated multilayer film has not observed any breakage and cracks in the multilayer film. Figure 4 SEM cross-sectional view of Co / Pd multilayer fil...

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Abstract

The invention discloses palladium plating liquid which can form steady Co / Pd nano multilayer films, the thickness of the palladium films is at nano level, and palladium deposition is bright and has no crack. The palladium plating liquid comprises 0.1 to 30g / l of dissolvable palladium salt calculated in Pd with the improvement of adding 0.01 to 1g / l of pyridine sulfonate or the salt, 0.005 to 1g / l of cerium salt calculated in Ce, 30 to 100ml / l of ethylene diamine and 20 to 200g / l of conductive salt, and the PH value of the plating liquid is 7 to 12. The palladium plating liquid of the Co / Pd nano multilayer films prepared by improved electro-crystallization has excellent storage stability, and the surface of the plating layer is smooth, compact and shiny. No crack occurs even the plating layer is amine-exposed for 24 hours at room temperature. Furthermore, the Co / Pd nano multilayer films have clear and continuous layer structure, and the coercive force of the multilayer films can reach 1130Oe, thus electro-crystallizing excellent Co / Pd multilayer films.

Description

technical field [0001] The present invention relates to a kind of palladium plating liquid that is applied to Co / Pd multi-layer film by electrocrystallization of double groove method, more specifically a kind of can make Co / Pd multi-layer film shedding problem be solved and change its luster effect, A palladium plating solution that forms a stable nano-multilayer film deposit with high magnetic properties. Background technique [0002] The nano-multilayer film composed of magnetic layer and non-magnetic layer has excellent magnetic properties and physical properties, such as the giant magnetoresistance effect (GMR) and the change of easy magnetic direction, etc. The research on its properties is not only of great significance in magnetic theory, And it is expected to be applied to magnetically sensitive devices and increase the magnetic recording density, etc. Therefore, the research on different multilayer film systems has aroused great interest of scholars from all over th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D3/52H01F41/26H01F10/00
Inventor 曹为民陈浩吕春雷印仁和石新红
Owner SHANGHAI UNIV
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