Chemical plating repairing method for palladium or palladium alloy composite film

A technology of electroless plating and palladium alloy, which is applied in the direction of liquid chemical plating, chemical instruments and methods, membrane technology, etc., can solve the problems of no catalytic activity of electroless plating, decreased repair effect, and membrane rupture, so as to speed up the speed of palladium plating, Improved hydrogen permeation performance and high membrane density

Active Publication Date: 2010-07-21
RISON HI TECH MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above membrane repair methods gradually shrink the cavity by promoting the growth of the metal layer at the edge of the membrane defect, but as the pore size of the membrane defect further decreases, the repair effect will gradually decrease
In addition, the method of filling film defects with fillers such as ceramic powders, polymer materials, and colloids, and then performing electroless plating has also been reported. However, these materials themselves have no catalytic activity for electroless plating, and the matrix material needs to be activated again; activation When the surface of the entire palladium membrane will form a colloidal activation layer, it will form a sandwich layer in the palladium membrane when the electroless plating is continued, and the membrane will be ruptured and polluted after being heated.

Method used

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  • Chemical plating repairing method for palladium or palladium alloy composite film
  • Chemical plating repairing method for palladium or palladium alloy composite film
  • Chemical plating repairing method for palladium or palladium alloy composite film

Examples

Experimental program
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Effect test

Embodiment 1

[0022] (1) The sample used is a defective pure metal palladium membrane tube with an outer diameter of 1.2cm, an inner diameter of 0.7cm, a length of 8.4cm, and a film thickness of 2.5μm. The matrix material is porous Al 2 o 3 . The nitrogen flux is 25 mL / min at a pressure of 1 bar.

[0023] (2) The repair fluid uses Pd(OH) with a palladium ion content of 0.001mol / L 2 For the colloid, refer to the patents of Huang Yan and others for the specific preparation method (Huang Yan, Fan Jingjing, Shu Shili, Hu Xiaojuan. An activation process for non-metallic substrate electroless plating. Chinese patent ZL200710022996.6, 2007).

[0024] (3) Repair operations such as figure 2 shown. The two ends of the membrane tube are sealed with silica gel plugs, and the upper end is connected with a vacuum pump, wherein the inner tube penetrates into the vicinity of the bottom of the membrane tube. Immerse the membrane tube in the repair fluid and vacuumize it, and stop the operation as soon...

Embodiment 2

[0028] (1) The matrix material used is Al with an outer diameter of 1.2cm, an inner diameter of 0.75cm, a length of 8.5cm, and an average pore diameter of 0.2μm. 2 o 3 porous ceramic tube. It was washed successively with commercially available detergent solution, tap water, and deionized water. The matrix tube is filled with a soft silicone rubber rod.

[0029] (2) Substrate pretreatment adopts conventional sensitization-activation method. Sensitization solution formula is: SnCl 2 5g / L, concentrated hydrochloric acid 1mL / L; activation solution formula: PdCl 2 0.2g / L, concentrated hydrochloric acid 1mL / L. Dip the substrate in the sensitizing solution and rinse it with deionized water, then dip it in the activation solution and rinse it. Repeat the sensitization-activation operation 4 times, and the surface of the substrate is dark brown.

[0030] (3) Electroless palladium plating. The conditions are the same as step (4) of Example 1, and the thickness of the palladium ...

Embodiment 3

[0036] (1) The sample used is a palladium-silver alloy film tube with relatively large defects, with an outer diameter of 1.2 cm, an inner diameter of 0.8 cm, a length of 8.2 cm, and a film thickness of about 4 μm. Its nitrogen flux is 85 mL / min at a pressure of 1 bar.

[0037] (2) The repair fluid is 2mol / L AgNO 3 solution.

[0038] (3) With the step (3), (4) of embodiment 1.

[0039] (4) The film thickened by 0.8 μm after repair. The membrane tube was alloyed at 650°C for 12 hours under a hydrogen atmosphere, and the nitrogen flux was reduced to 10mL / min at a pressure of 0.1MPa.

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Abstract

The invention relates to a chemical plating repairing method for a palladium or palladium alloy composite film. A solution or colloid of a metallic compound is used as a repairing liquid which is dipped into a film defect through capillary force and suction force and reduced to form metal particles that are filled into the defect, then a metal eliminating film is deposited by using a chemical plating method, wherein the metal particles play a role of a catalyst to the chemical plating. The method can be used for repairing the film, and can be alternated with the preparation process of the film, thereby realizing higher film compactness under the condition of same film thickness, or enabling the film to be thinner under the condition of film compactness, greatly improving the hydrogen penetrating property of the film and realizing higher hydrogen purity.

Description

Technical field: [0001] The invention relates to an electroless plating repair method of a palladium or palladium alloy composite membrane, which is used for improving the selectivity of the membrane and obtaining higher hydrogen separation effect. Background technique: [0002] Hydrogen separation is a key technology in the production and recovery of hydrogen. Practical separation methods mainly include pressure swing adsorption (PSA), deep cooling (Deep cooling), temperature swing adsorption (TSA), membrane separation, etc. Among them, the membrane separation method is especially suitable for small and medium-scale, especially small-scale hydrogen separation, and has the outstanding advantages of simple operation and low investment. In recent years, countries around the world have attached great importance to hydrogen energy, which has also played a huge role in promoting the development of hydrogen membrane separation technology. Hydrogen permeable membrane is the key ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C18/44C23C18/34C23C18/18
CPCC23C18/44C23C18/34B01D71/022C23C18/1837B01D65/108
Inventor 黄彦魏娟胡小娟陈卫东
Owner RISON HI TECH MATERIALS CO LTD
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