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Method for preparing metallic complex film

A technology of metal composite and porous composite membrane, which is applied in the direction of metal material coating process, superimposed layer plating, liquid chemical plating, etc., can solve the problem of easy formation of pinholes and cracks, low selectivity, and porous bottom membrane Problems such as large average pore size, to achieve the effect of improving roughness and improving pore structure

Active Publication Date: 2008-03-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Their common features are: the use of conventional SnCl 2 and PdCl 2 Solution sensitization - chemical plating with vacuum suction after activation, through the action of vacuum suction, the speed of chemical plating is accelerated, and the partially reduced Pd grains enter the pores of the porous bottom film, strengthening the metal layer and the bottom film. However, due to the large average pore size of the porous bottom film used, it is difficult to form a uniform and dense metal film, and the metal deposition speed is too fast, and the gas (bubbles) generated by electroless plating cannot be removed in time to easily form pinholes and cracks. Deficiency, the permeation amount that causes the prepared palladium composite membrane and palladium alloy composite membrane is low, and selectivity is not high (generally H 2 / N 2 The selectivity is several hundred), and it is not suitable for the practical requirements of the industry

Method used

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  • Method for preparing metallic complex film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take PURAL SB powder (a kind of commercial pseudo-boehmite for industrial use produced by Germany Condea company) as raw material to prepare 0.5mol / L γ-AlOOH sol, add 1.2wt%PVA and 0.6wt%PVA in γ-AlOOH sol PEG to adjust the viscosity of the sol, mixed evenly to form a dip-coating sol. Immerse the cleaned porous ceramic bottom film tube (bottom film thickness 5mm, average pore diameter 0.3μm, porosity about 40%) in the above-mentioned dip coating sol, dip coating for 15 seconds, dry at room temperature for two days, and place in a muffle furnace Calcined at 500-600°C for 3 hours, the surface pre-modified porous asymmetric bottom membrane can be obtained, the thickness of the top layer is about 3 μm, and the average pore diameter is 7.5nm. Subsequently, EDTA and PdCl 2 (1:1 molar ratio) made into solution so that Pd 2+ Chelation with EDTA to produce [PdEDTA] 2- , take the above solution and add it to 0.5mol / L gamma-AlOOH sol (Pd / Al=4.8 / 1000 molar ratio), and add 1.6wt%...

Embodiment 3

[0038] As described in Example 1, first carry out vacuum chemical palladium plating on the reduced film tube, change the plating solution after rinsing and carry out vacuum chemical copper plating, while maintaining a certain vacuum degree (P A =91KPa, P B =3KPa, absolute pressure), the composition of electroless copper plating solution is: CuCl 2 .2H 2 O (8.6g / L), Na 2 EDTA.2H 2 O (19.2g / L), KNaC 4 h 4 o 6 (11.3g / L), NaOH (18.0g / L), K 4 Fe(CN) 6 .3H 2 O (mg grade), 2,2-bipyridine (mg grade), N, N, N', N'-tetramethylethylenediamine (mg grade), HCHO (≥36wt%) (14ml / L), The pH value is 13.5, the constant temperature is 30°C, and the vacuum electroless plating is carried out with stirring. Control the vacuum electroless plating time, palladium plating 15-30min, copper plating 10-30min (palladium, copper are different in deposition rate in vacuum electroless plating, therefore provide the time frame of a vacuum electroless plating here. And the palladium-copper alloy film...

Embodiment 4

[0040] As described in Example 3, the vacuum chemical plating time is controlled, palladium plating is 30-60min, copper plating is 10-50min, and the vacuum chemical plating has prepared a Pd-Cu alloy film with a thickness of about 8 μm. When the pressure difference is 1bar at 500°C, hydrogen Maximum penetration is 15m 3 / m 2 .h, H 2 / Ar selectivity is greater than 3000, in the temperature range of 500-200 ° C in different proportions of H 2 / Ar mixed gas atmosphere for 30 days, the gas permeability remains stable, which indicates that the alloy membrane can overcome the hydrogen embrittlement of pure palladium membrane, and expand the temperature range of the hydrogen separation application of the membrane.

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Abstract

The vacuum chemical plating process for preparing composite metal film includes the first pre-modification of porous film by means of sol-gel technology to introduce one transition layer containing metal crystal seed with self-catalytic reduction activity to the chemical plating, and the subsequent vacuum chemical plating by means of forming different vacuum degrees on two sides of the modified porous composite film. The process can raise the hydrogen permeating performance of the composite metal film and raise the stability of the composite metal film.

Description

technical field [0001] The present invention relates to the preparation of metal composite membranes. Specifically, it provides a porous composite membrane containing metal active components prepared by in-situ modification of the surface of colloidal sol particles and introducing metal seeds as the base membrane. A new method for preparing metal composite films by plating. Background technique [0002] As an important chemical and chemical raw material, hydrogen has been in increasing demand in the fields of electronics, metallurgy and petrochemicals in recent years. At the same time, with the rise of fuel cells, especially the continuous development of proton exchange membrane fuel cells, hydrogen as a How to efficiently separate and purify hydrogen has become a key technology. Dense palladium membranes and palladium alloy membranes have been paid more and more attention due to their completely selective hydrogen permeation properties, and have broad application prospects...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C28/00C23C18/00
Inventor 熊国兴张小亮杨维慎刘杰盛世善
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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