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Si-containing nanometer porous Pd material and preparation method thereof

A nano-porous, high-content technology, which is applied in the direction of electrical components, circuits, battery electrodes, etc., can solve the problems that hinder the practical application of nano-porous materials, the difficulty of testing related properties of nano-porous structures, and fragility, and achieve uniform pore size. control, excellent catalytic performance, and good structural integrity

Inactive Publication Date: 2016-08-31
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, nanoporous metals such as Au, Cu, and Pt are prepared by dealloying in alloy systems such as Ag-Au, Cu-Au, Al-Au, Mn-Cu, Si-Pt, and Cu-Pt, but The prepared nanoporous material samples generally have shortcomings such as fragility, cracking, poor structural integrity, and easy size coarsening, which makes it difficult to test the relevant properties of nanoporous structures, and the reproducibility is poor, which seriously hinders related nanoporous materials. Practical application of porous materials

Method used

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  • Si-containing nanometer porous Pd material and preparation method thereof
  • Si-containing nanometer porous Pd material and preparation method thereof
  • Si-containing nanometer porous Pd material and preparation method thereof

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preparation example Construction

[0017] The first is the preparation of precursor alloy strip samples, which includes three steps: raw material proportion weighing, alloy ingot melting and strip sample preparation. The specific operation is as follows:

[0018] Step 1: Raw material ratio weighing

[0019] According to the chemical composition of the material Cu 1-x-y PD x Si y (10% ≤ x ≤ 30%, 0% < y ≤ 10%), select a suitable proportion of ingredients, convert according to the proportion and weigh the weight of each component raw material, ready to use. The purity of the metal raw materials used is: 99.99wt.% Cu, 99.5wt.% Pd and 99.999wt.% Si.

[0020] Step 2: Alloy ingot melting

[0021] The weighed raw materials of each component are mixed, placed in a water-cooled copper crucible of a non-consumable arc melting furnace, and smelted under the protection of high-purity argon, and the smelting is repeated three times to obtain an alloy ingot with a relatively uniform composition. The alloy mass loss rate...

Embodiment 1

[0040] Example 1Cu 75 PD 20 Si 5 alloy

[0041] Step 1: Weighing of component materials and melting of alloy ingot

[0042] Will Cu 75 PD 20 Si 5 The atomic percentage is converted into weight percentage, the ingredients are weighed, the weighed raw materials are mixed, placed in the water-cooled copper crucible of the non-consumable arc melting furnace, and arc melting is carried out under the protection of high-purity argon, and then the The alloy ingot is flipped up and down, and smelted repeatedly 3 times to obtain an alloy ingot with uniform composition.

[0043] Step 2: Preparation of strip samples

[0044] The alloy ingot obtained by smelting is crushed, put into a quartz tube with a nozzle size of 8 mm long × 1 mm wide, and then the quartz tube is placed in an induction heating coil for heating, and the molten alloy is blown out with high-purity argon to make it Spray on a high-speed rotating water-cooled copper roller with a linear speed of 40m / s to obtain all...

Embodiment 2

[0054] Example 2Cu 75 PD 24 Si 1 alloy

[0055] Step 1: Weighing of component materials and melting of alloy ingot

[0056] Same as Step 1 in Example 1.

[0057] Step 2: Preparation of strip samples

[0058] Same as Step 2 in Example 1.

[0059] Step 3: Analysis of the structure of the precursor alloy

[0060] With step 3 in embodiment 1, analysis result shows that Cu 75 PD 24 Si 1 The alloy is a nearly single FCC solid solution structure, the grain size is about 0.5-4μm, and there are very few Si-rich precipitates on the grain boundaries.

[0061] Step 4: Electrochemical performance test and dealloying experiment

[0062] Using Gamry Interface 1000 electrochemical workstation, in 0.5mol / L H 2 SO 4 solution, for Cu 75 PD 24 Si 1 The room temperature electrochemical performance evaluation of alloy strips (scanning rate is 1mV / s), the measured critical potential is about 1.4V (experimental reference electrode is Ag / AgCl electrode, the same below), which is higher ...

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Abstract

The invention discloses a Si-containing nanometer porous Pd material and a preparation method thereof and belongs to the technical field of new materials. The nanometer porous Pd material contains Cu, Si and Pd elements; the chemical constitution of alloy of a precursor of the nanometer porous Pd material is Cu<1-x-y>Pd<x>Si<y>, wherein x and y represent atomic percent, x is not smaller than 10% and not larger than 30%, and y is larger than 0% and smaller than or equal to 10%; according to difference of the alloy ingredients of the precursor, the bore diameter and the ligament diameter can be controlled between 2 to 20 nanometers. The preparation method comprises the following steps: performing non-consumed electric arc melting in combination with a water-cooling copper roller melt rapid quenching technique to prepare a Cu-Pd-Si solid solution alloy precursor wide strip material; by taking the strip material as a working electrode, performing electrochemical dealloying under a room-temperature weak acid environment to obtain the nanometer porous Pd material. The nanometer porous Pd material is low in cost, simple in preparation process, complete and free of cracks in structure and uniform and controllable in pore size, and has an excellent catalytic performance on electro-oxidation reaction of organic small molecules such as methanol in an alkaline solution. The nanometer porous Pd material can be used as an anodic reaction catalyst for a fuel battery such as alkaline ethanol or is directly used as an anode supporting material.

Description

technical field [0001] The invention relates to a Si-containing nanoporous Pd material and a preparation method thereof, belonging to the technical field of new materials. Background technique [0002] Nanoporous metals are composed of nanoscale pores and metal ligaments, which have the characteristics of high specific surface area, high porosity, volume effect, surface effect, quantum size effect, etc., and have high electrical conductivity, thermal conductivity and good mechanical properties of metal materials , they have important application prospects in the fields of filtration, surface catalysis, sensing, and drug delivery. [0003] The preparation methods of nanoporous metals mainly include powder sintering method, colloidal crystal template method, oblique incidence deposition method and dealloying method. Among them, the dealloying method is widely used due to its simple process and high preparation efficiency. At present, nanoporous metals such as Au, Cu, and Pt ...

Claims

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Application Information

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IPC IPC(8): C22C3/00C22C5/04H01M4/92
CPCC22C3/00C22C5/04H01M4/92Y02E60/50
Inventor 王英敏羌建兵梁靖王清董闯
Owner DALIAN UNIV OF TECH
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