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Gradient palladium-yttrium hydrogen-permeating composite film material and preparation method thereof

A composite film, hydrogen permeation technology, applied in metal material coating process, ion implantation plating, coating and other directions, can solve the problem of unable to maintain stability and mechanical strength, affecting the hydrogen permeation capacity of pure palladium membrane, reducing membrane hydrogen permeation rate and other problems, to achieve the effect of low cost, strong practicability, and reduction of micro-cracks

Inactive Publication Date: 2018-07-20
SHANDONG JIANZHU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Both the α-hydrogen-poor phase and the β-hydrogen-rich phase are face-centered cubic lattices, but the lattice constant of the β-hydrogen-rich phase will increase (the lattice constant will increase by 3.5% in pure hydrogen), resulting in the existence of a palladium layer Defects such as poor adhesion and high brittleness are the so-called "hydrogen embrittlement", which significantly affects the hydrogen permeability of pure palladium membranes
However, since the thickness of the palladium film is generally around 50-100 μm, it cannot maintain sufficient stability and mechanical strength if it is too thin, and it will greatly increase the cost and reduce the hydrogen permeability of the film if it is too thick.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: The gradient palladium yttrium hydrogen permeable composite thin film material adopts the following specific process.

[0029] (1) Place the brightly polished yttrium target and palladium target on the two DC sputtering target positions of the high vacuum magnetron sputtering system; adjust the distance between the center of the plane where the yttrium target is located and the center of the deposition sample stage to be 8 cm, The distance between the center of the plane where it is located and the center of the deposition sample stage is 4 cm, which remains unchanged during the co-sputtering process.

[0030] (2) Cut the purchased commercial copper foil into a size of 5 cm × 5 cm as the substrate. The copper foil substrate was ultrasonically cleaned with acetone for 5 minutes to remove residual organic matter on the surface, and then ultrasonically cleaned with dilute hydrochloric acid for 5 minutes to remove surface oxides. Finally, Use absolute ethanol ...

Embodiment 2

[0036] Embodiment 2: The gradient palladium yttrium hydrogen permeable composite thin film material adopts the following specific process.

[0037] (1) Place the brightly polished yttrium target and palladium target on the two DC sputtering target positions of the high-vacuum magnetron sputtering system; The distance between the center of the plane and the center of the deposition sample stage is 6 cm, which remains unchanged during the co-sputtering process.

[0038] (2) The soda-lime glass substrate was ultrasonically cleaned with acetone for 5 min to remove residual organic matter on the surface, and then absolute ethanol was used to remove residual solution ions on the surface and dried quickly.

[0039] (3) Transfer the soda-lime glass substrate to the center of the substrate sample stage of the magnetron sputtering equipment, fix it with double-conducting copper foil tape, close the magnetron sputtering reaction chamber, and perform vacuuming operation.

[0040] (4) Pum...

Embodiment 3

[0044] Embodiment 3: The gradient palladium yttrium hydrogen permeable composite thin film material adopts the following specific process.

[0045] (1) Place the brightly polished yttrium target and palladium target on the two DC sputtering target positions of the high-vacuum magnetron sputtering system; adjust the distance between the center of the plane where the yttrium target is located and the center of the deposition sample stage to be 9 cm, and the palladium target The distance between the center of the plane and the center of the deposition sample stage is 5 cm, which remains unchanged during the co-sputtering process.

[0046] (2) Cut the purchased commercial copper foil into a size of 10 cm × 10 cm as the substrate. The copper foil substrate was ultrasonically cleaned with acetone for 5 minutes to remove residual organic matter on the surface, and then ultrasonically cleaned with dilute hydrochloric acid for 5 minutes to remove surface oxides. Finally, Use absolute e...

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Abstract

The invention discloses a gradient palladium-yttrium hydrogen-permeating composite film material and a preparation method thereof. The preparation method takes a commercial copper foil or soda-lime glass as a substrate, a high-purity palladium target and a high-purity yttrium target as sputtering materials, and high vacuum multi-target magnetron sputtering equipment as a preparation tool, and by fixing the target position sputtering power of the yttrium target, changing the target position sputtering power of the palladium target in a co-sputtering deposition process, the adjustment on the yttrium and palladium relative content in the film material is achieved, and the thickness of the prepared film is controlled by changing the co-sputtering time, so that the palladium-yttrium hydrogen-permeating composite film material with the changeable thickness is prepared finally. The preparation method has the characteristics that the preparation flow is short, the operation is simple, the parameter control range is wide, the implementation is easy, the gradient layer thickness and palladium and yttrium relative content can be flexibly controlled, and the preparation method has good commercial prospects.

Description

technical field [0001] The invention relates to the field of preparation of gradient thin film materials, in particular to a gradient palladium yttrium hydrogen permeable composite thin film material and a method for preparing the thin film material by high-vacuum double-target magnetron sputtering. Background technique [0002] Palladium has excellent hydrogen-sensing properties, and is often used as the hydrogen-sensing layer of hydrogen-sensing sensors, and most of the hydrogen-sensing elements currently use this metal. by Pd-H 2 It can be seen from the phase diagram of the system that below 300 °C, palladium exists in two forms: α phase and β phase. In the absence of hydrogen, palladium always exists in the form of α-hydrogen-poor phase; but when the hydrogen content in palladium exceeds the limit of hydrogen absorption of α-phase palladium, palladium will undergo a phase transition, from α-hydrogen-poor phase into a β-hydrogen-rich phase. Both the α-hydrogen-poor pha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C14/35C23C14/18C23C14/16C23C14/58
CPCC23C14/352C23C14/165C23C14/185C23C14/5806
Inventor 张昌钦其他发明人请求不公开姓名
Owner SHANDONG JIANZHU UNIV
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