Chemical plating method for preparing ultrathin palladium film with high specific surface area

An electroless plating and palladium film technology, which is applied in the field of electroless plating of ultra-thin palladium-based composite films, can solve the problems of difficult control of etching process corrosion thickness, affecting bonding strength, cumbersome process, etc., and achieve enhanced hydrogen permeability and surface activity , reduce waste of resources, simple process effect

Inactive Publication Date: 2011-04-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition to the cumbersome process of these methods, the etching process is difficult to control the thickness of the corrosion, which will form perforations at the thin layer of the film surface; metal thermal diffusion will inevitably leave metal impurities in the bulk phase of the palladium film; and oxidation will destroy the metal. The bonding between the film layer and the carrier interface, thus affecting the bonding strength between the two

Method used

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  • Chemical plating method for preparing ultrathin palladium film with high specific surface area
  • Chemical plating method for preparing ultrathin palladium film with high specific surface area
  • Chemical plating method for preparing ultrathin palladium film with high specific surface area

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Preparation of palladium / ceramic composite membrane (inert gas driven reducing agent)

[0020] 1. Plating solution preparation

[0021] 1) Preparation of palladium metal complex solution. Weigh 1.86g disodium edetate and dissolve it in 100ml water, then measure PdCl separately 2 Solution (20g Pd / l) 25ml, NH 3 h 2 O (28%) 120ml was poured into the beaker of EDTA aqueous solution successively, diluted to 500ml, pH value 11-12, stirred gently for 1 hour (h).

[0022] 2) Preparation of reducing agent solution. Dilute hydrazine hydrate to 0.65mol / l for later use.

[0023] 2. Electroless plating

[0024] 1) Activate the seed nucleus. The ceramic carrier was successively immersed in the dilute solution of the activation solution OPC-50Inducer and the reducing agent OPC-150Cryster MU (Okuno Chemical Industry Co., Ltd., Japan) to activate the seed nucleus, and circulated until the surface became uniform dark gray. In order to make the distribution of palladium nuclei on ...

Embodiment 2

[0031] Preparation of palladium / ceramic composite membrane (osmotic pressure driven reducing agent)

[0032] 1. Plating solution preparation

[0033] Do not add EDTA in the plating solution, add NaCl 88g, other with example 1.

[0034] 2. Electroless plating

[0035] 1) Activate the seed nucleus. With embodiment 1.

[0036] 2) Chemical spot plating. Dip the pre-plated ceramic tube in the plating solution, the plating solution is weakly stirred, and the plating temperature is 50°C. Take diluted N 2 h 4 10ml of aqueous solution (0.65mol / l) was injected into the ceramic tube, and removed after electroless plating for 3 hours.

[0037] After the electroless plating is completed, after cleaning and drying, the palladium ceramic composite membrane is annealed at 500° C. under a hydrogen atmosphere for 40 hours. By the weight difference before and after electroless plating, the average film thickness of the obtained palladium film is 1.8 μm. According to the characterization ...

Embodiment 3

[0041] Preparation of Pd-Ag / Ceramic Composite Membrane

[0042] 1. Plating solution preparation

[0043] 1) Preparation of palladium-silver metal complex solution. Plating solution configuration is the same as that of Example 1, additionally adding AgNO 3 Solution (20g / l) 2ml.

[0044] 2) Preparation of reducing agent solution. With embodiment 1.

[0045] 2. Electroless plating

[0046] 1) Activate the seed nucleus. With embodiment 1.

[0047] 2) Chemical spot plating. The pre-plated ceramic carrier is immersed in the plating solution, the plating solution is weakly stirred, and the plating temperature is 58°C. Reductant N 2 h 4 10ml of aqueous solution was poured into the ceramic tube, and the upper end of the tube was connected to the pressurized system and sealed with polytetrafluoroethylene. After 60 minutes without loading pressure, pressurize to 2kPa, after 120 minutes, increase the pressure to 5kPa, take out after 60 minutes of reaction.

[0048] After the e...

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Abstract

The invention relates to a chemical plating method for preparing a palladium film or a palladium and silver alloy film, which comprises the following steps of: dividing plating solution of palladium salt complex or plating solution of palladium and silver amine salt complex into two parts by utilizing a porous carrier, adding a reducing agent to the plating solution at one side, making the reducing agent have self catalytic reaction with palladium salt complex or palladium and silver amine salt complex in the plating solution through holes and flaws, and forming a palladium film at one side of the porous carrier, which comes into contact with the palladium salt complex or the palladium and silver amine salt complex. High specific surface area can be obtained with the chemical plating method without any extra complicated processing, and the hydrogen permeation properties and the surface activity of the film can be enhanced. The palladium film prepared with the method is ultrathin, so resource waste can be reduced. Besides, the invention also has the advantages of simple technique, simple equipment and economic investment saving.

Description

technical field [0001] The invention relates to the preparation of electroless plating of a palladium (alloy) / porous carrier composite membrane, and specifically provides an electroless plating method for preparing an ultra-thin palladium-based composite membrane with a high specific surface area. technical background [0002] Dense palladium and its alloy membranes have selective permeation properties for hydrogen and catalytic properties for many dehydrogenation reactions. Therefore, they have broad application prospects in the fields of hydrogen separation, hydrogen purification and hydrogen-related membrane reactions. The early palladium and palladium alloy films were unsupported and usually prepared by cold rolling, so the thickness of these palladium and palladium alloy films was generally greater than 200 μm. Since the rate of hydrogen permeation through palladium and palladium alloy films is inversely proportional to the film thickness, the hydrogen permeation rates ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C18/42
Inventor 徐恒泳曾高峰史蕾安德里斯·歌德巴赫
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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