Method for preparing palladium nanometer sheet with optical property

A palladium nano and flake technology, applied in the field of preparation of palladium nano materials, can solve the problems such as difficult control of the formation and growth of nano crystal nuclei on the surface of the substrate, uncontrollable particle size of nano gold, cumbersome product purification process, etc. Large-scale production, easy operation and high yield

Inactive Publication Date: 2012-10-03
ANHUI UNIV OF SCI & TECH
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Problems solved by technology

The hydrothermal synthesis method is carried out under high temperature and high pressure, and the reaction conditions are relatively harsh; the polyhydric reduction method introduces more additives, and even uses the organic phase as a solvent. Not only is the product purification process cumbersome, it may also bring certain environmental pollution problems. It is not conducive to large-scale industrial production; the ascorbic acid reduction method is relatively simple, without heating, it only needs to add ascorbic acid to the palladium precursor aqueous solution and stir. The reaction has the advantages of fast, simple and good reproducibility, but the biggest limitation of this method is The reaction speed is too fast, so the particle size of the prepared nano-gold is uncontrollable
[0005] 2. Seed crystal method. The biggest advantage of this method is that it avoids secondary nucleation, and it is easy to obtain nanoparticles with different shapes and sizes. However, this method is mainly reflected in several steps. First, the seed crystal is synthesized, and then Initiating nucleation further, resulting in the reaction cannot be completed in one step, and the operation steps are complicated
[0006] 3. Electrochemical deposition method, which is a method for preparing nanoparticles by inducing a chemical reaction in an electrolyte solution by an external electric field. This method is an economical deposition method and is easy to operate, but it is harmful to the generation of nanocrystal nuclei on the surface of the substrate and Growing up is difficult to control
However, the palladium nanoparticle size prepared by this method is below 10nm, the plasmon resonance absorption peak is around 220nm, and there is no optical property in the band above 300nm. Questions about the micromechanism of reactions catalyzed by palladium nanomaterials present challenges

Method used

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  • Method for preparing palladium nanometer sheet with optical property
  • Method for preparing palladium nanometer sheet with optical property
  • Method for preparing palladium nanometer sheet with optical property

Examples

Experimental program
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Embodiment 1

[0041] 1. Add 20mL water and 4mL ethanol in turn to the reaction vessel, and stir to obtain a water-ethanol mixed solution system;

[0042] 2. Set the final concentration to 7.04×10 -4mol / L of PdCl 2 Powder and 1.49×10 -2 Add mol / L CTAB to the water-ethanol mixed solution system, put the prepared solution on a constant temperature magnetic stirrer at 25°C and stir for 2 hours, the color of the solution is light yellow;

[0043] 3. Put the uniformly stirred reaction solution in a self-designed light reaction box, and place it under a 60W ordinary commercially available incandescent light for 6 hours in parallel;

[0044] 4. The obtained black precipitate was separated by centrifugation, washed once with ethanol and acetone, and dried in a vacuum oven at 40° C. for 24 hours to obtain a palladium nanosheet material.

[0045] 5. The X-ray diffraction (XRD) pattern of the sample is measured by Beijing Puxi General Instrument Co., Ltd. XD-3 X-ray diffraction analyzer (Cu target, ...

Embodiment 2

[0048] 1. Add 20mL water and 4mL ethanol in turn to the reaction vessel, and stir to obtain a water-ethanol mixed solution system;

[0049] 2. Set the final concentration to 7.04×10 -4 mol / L of PdCl 2 Powder and 7.04×10 -4 Add mol / L CTAB to the water-ethanol mixed solution system, put the prepared solution on a constant temperature magnetic stirrer at 25°C and stir for 2 hours, the color of the solution is light yellow;

[0050] 3. Put the evenly stirred reaction solution in a self-designed light reaction box, and place it under a 60W incandescent light for 6 hours in parallel;

[0051] 4. The obtained black precipitate was separated by centrifugation, washed once with ethanol and acetone, and dried in a vacuum oven at 40° C. for 24 hours to obtain a palladium nanosheet material.

[0052] 5. The microscopic morphology of the nano-palladium flake material is as follows: image 3 As shown, the morphology of palladium nanoflakes is mostly hexagonal, the particle size distribu...

Embodiment 3

[0054] 1. Add 20mL water and 4mL ethanol in turn to the reaction vessel, and stir to obtain a water-ethanol mixed solution system;

[0055] 2. Set the final concentration to 7.04×10 -4 mol / L of PdCl 2 Powder and 5.64×10 -2 Add mol / L CTAB to the water-ethanol mixed solution system, put the prepared solution on a constant temperature magnetic stirrer at 25°C and stir for 2 hours, the color of the solution is light yellow;

[0056] 3. Put the uniformly stirred reaction solution in a self-designed light reaction box, and place it under a 60W ordinary commercially available incandescent light for 6 hours in parallel;

[0057] 4. The obtained black precipitate was separated by centrifugation, washed once with ethanol and acetone, and dried in a vacuum oven at 40° C. for 24 hours to obtain a palladium nanosheet material.

[0058] 5. The microscopic morphology of nano-palladium materials is as follows: Figure 4 As shown, the morphology of palladium nanoflakes is triangle, rhombus...

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Abstract

The invention relates to a method for simply preparing a palladium nanometer sheet with an optical property. The method comprises the following steps of: adding PdCl2 powder with an equivalent concentration of 7.04*10<-4>mol / L and hexadecyl trimethyl ammonium bromide with an equivalent concentration of 7.04*10<-4> to 5.64*10<-2>mol / L into a water-ethanol mixed solution system; stirring the prepared solution, wherein the solution is light yellow; irradiating the reaction system under a 15-200W incandescent lamp for 1 to 12 hours; stopping the irradiation; performing centrifugal separation to obtain black precipitates; washing for one time by using ethanol and acetone respectively; and drying into a vacuum drying oven at the temperature of 40 DEG C, and thus obtaining a palladium nanometer sheet material. The particle size of the nanometer material obtained by the method is 28 to 44 nanometers, particles are polygonal, and the sheet is wide in particle size distribution; and an ultraviolet-visible extinction spectrum appears near 340 nm, so that the nanometer material has the optical property in the area. The preparation method is mild in condition, simple in process, short in production period and easy to produce on a large scale.

Description

technical field [0001] The invention relates to a preparation method of palladium nanometer material. Background technique [0002] Palladium nanomaterials have attracted much attention as good hydrogen storage materials, conductive pastes, especially heterogeneous catalytic materials. Because the properties of palladium nanostructures are closely related to their size and shape, it is particularly important to develop facile synthesis methods with controllable size and shape. At present, researchers can synthesize palladium nanomaterials with different sizes and shapes and multifunctionality through a variety of physical, chemical and biological methods. Since chemical synthesis operates on substances at the molecular level, good chemical uniformity can be obtained, and the solution reaction method is easier to control the particle size, so the preparation of metal palladium nanomaterials is currently widely used in liquid-based chemical methods. [0003] The main chemica...

Claims

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Application Information

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IPC IPC(8): B22F9/24
Inventor 王艳丽谭德新张明旭张宏艳晏莹史丽丽陈凤
Owner ANHUI UNIV OF SCI & TECH
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