Gold deposition process on surface of metal palladium and preparation of palladium alloy membrane

A technology of alloy membrane and palladium membrane, which is applied in the field of metal membrane, can solve problems such as segregation of alloy membrane and affect membrane hydrogen separation performance, and achieve the effect of high hydrogen purification ability, reduced volatilization, and uniform gold coating

Active Publication Date: 2017-02-08
RISON HI TECH MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] (4) The thickness distribution of the gold layer should be uniform, otherwise the final composition of the alloy film will be segregated, which will affect the hydrogen separation performance of the film
However, traditional electroless gold plating is mainly for anti-corrosion, decoration, electrical conductivity and other purposes, and may not be suitable for the preparation of Pd-Au alloy films, or may not be able to guarantee the hydrogen permeability, selectivity, and stability of Pd-Au alloy films. high standard requirements

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The raw palladium film was provided by Nanjing Gaoqian Functional Materials Technology Co., Ltd. It is a pure metal palladium film supported on a porous stainless steel substrate. It is prepared by chemical plating. The outer diameter is 12mm, the inner diameter is 10mm, the length is 75mm, and the thickness of the palladium metal layer is 5μm. The palladium membrane was washed with deionized water.

[0026] (1) Preparation of gold plating solution. Prepare HAuCl with a concentration of 1 mmol / L 4 solution. Preparing Na 2 EDTA 0.16mol / L, NH 3 ·H 2 A mixed solution of O (concentrated ammonia 28%) 100ml / L and NaOH 0.2mol / L.

[0027] (2) Electroless gold plating. Mix the above two solutions in equal volumes before gold plating, put the cleaned raw palladium film into the gold plating solution, and slowly add 0.5mol / L N 2 H 4 solution. The pH of the solution is greater than 13, and the reaction temperature is normal temperature. The Au conversion rate was found to...

Embodiment 2

[0031] The raw palladium membrane is a pure metal palladium membrane supported on a porous ceramic substrate, prepared by chemical plating, with an outer diameter of 13 mm, an inner diameter of 8 mm, a length of 75 mm, and a palladium metal layer thickness of 5 μm. The palladium membrane was washed with deionized water.

[0032] (1) Preparation of gold plating solution. Prepare KAuCl with a concentration of 20 mmol / L 4 solution. formula K 2 EDTA 0.6mol / L, NH 3 ·H 2 Mixed solution of O (concentrated ammonia 28%) 400ml / L and KOH 2mol / L.

[0033] (2) Electroless gold plating. Mix the above two solutions in equal volumes before gold plating, put the cleaned raw palladium film into the gold plating solution, and slowly add 0.1 mol / L N 2 H 4 solution. The solution pH=14 and the reaction temperature was 35°C. The Au conversion rate was 97.9% by the weighing method, and the Pd / Au mass ratios of the prepared membranes were 97 / 3, 91 / 9, 84 / 16, and 79 / 21. The prepared membranes ...

Embodiment 3

[0037] The raw material palladium membrane is the same as in Example 1.

[0038] (1) with step (1) of embodiment 1. Prepare NaAuCl with a concentration of 10 mmol / L 4 solution. Preparing Na 2 EDTA0.3mol / L, NH 3 ·H 2 Mixed solution of O (concentrated ammonia 28%) 200ml / L and NaOH 1mol / L.

[0039] (2) with step (2) of embodiment 1. Put the cleaned raw palladium film into the gold plating solution, slowly add 0.2mol / L N 2 H 4 solution. The pH of the solution was 14, and the reaction temperature was 30°C. The Au conversion rate was found to be 99.1% by the weighing method, and the Pd / Au mass ratio of the prepared membrane was 88 / 12. The prepared membrane was washed and dried.

[0040] (3) Alloying. The as-prepared films were alloyed in N 2 The temperature was raised to 650°C at 2°C / min under the atmosphere, and then heated to 650°C under H 2 After holding for 4h in the atmosphere, switch to N 2 The atmosphere was cooled to room temperature.

[0041] (4) The obtained...

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Abstract

The invention relates to a method of preparing a Pd-Au alloy membrane by means of chemical plating on the surface of a porous ceramic or a porous metal matrix and belongs to the field of application of chemical plating. The method is characterized in that a gold plating solution used in a gold plating process for preparing the Pd-Au alloy membrane is composed of four agents: A, B, C and D, wherein A is one or more of chloroauric acid, gold chloride, sodium chloroaurate, potassium chloroaurate and ammonium chloraurate powder; B is a complexing agent EDTA, for example, Na2EDTA and (NH4)2EDTA; C is ammonia water; and D is NaOH or KOH. Compared with an existing gold plating method, the chemical plating process provided by the invention is mild in reaction condition and can be totally performed at normal temperature, and the gold plate is more uniform and compact, so that unordered gold precipitates are avoided and hollowness in a gold layer is avoided. As the gold chemical plating solution does not contain highly toxic cyanides, the process is an environmental-friendly green process. The gold plating process can improve the conversion rate and the utilization ratio of gold, and no impurities will be introduced into the gold plate.

Description

technical field [0001] The invention belongs to the field of metal films, and relates to a new method for preparing a Pd-Au alloy film, which is mainly used for separation and purification of hydrogen. Background technique [0002] Hydrogen has a wide range of uses in both industrial and civil fields. Many applications of hydrogen require high purity or strict restrictions on some sensitive impurities, so the separation and purification of hydrogen is crucial. Conventional hydrogen separation methods mainly include pressure swing adsorption, cryogenic and membrane separation. The former two are more suitable for medium and large-scale hydrogen separation, while membrane separation is the easiest to operate and is more suitable for small-scale hydrogen separation. The industrialized hydrogen separation membranes are polymer membranes and palladium membranes. The hydrogen separation capacity of polymer membranes is limited, and the purity of hydrogen production is not high, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C18/44
CPCC23C18/44
Inventor 黄彦李国峰
Owner RISON HI TECH MATERIALS CO LTD
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