Two-dimensional hollow palladium nanocrystal and preparation method thereof

A palladium nano and hollow technology is applied in the field of preparation of noble metal nano materials, which can solve the problems of high requirements for experimental environment and operation process, and achieve the effects of enhanced catalytic performance, low toxicity and mild reaction conditions.

Active Publication Date: 2015-06-24
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The palladium nanosheets synthesized by this method have high yield, uniform particle size, ultra-thin structure (about 1.8nm), large specific surface

Method used

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  • Two-dimensional hollow palladium nanocrystal and preparation method thereof
  • Two-dimensional hollow palladium nanocrystal and preparation method thereof
  • Two-dimensional hollow palladium nanocrystal and preparation method thereof

Examples

Experimental program
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[0042] Example 1

[0043] Step 1. Dissolve 16 mg of palladium acetylacetonate, 60 mg of cetyltrimethylammonium bromide, 100 mg of tungsten carbonyl, 90 mg of citric acid and 30 mg of polyvinylpyrrolidone in 10 mL of N,N dimethylformamide, and stir for 1 hour to make each The substance was fully dissolved, and the reaction solution was transferred to a 25 mL round bottom flask, and reacted at 80°C for 1 h. After the reaction is completed, the reaction solution is centrifuged to obtain hexagonal palladium nanosheets. Palladium nanosheets have morphology like figure 1 As shown, the thickness of the hexagonal palladium nanosheet is 1 nm, and the average side length is 15.7 nm.

[0044] Step 2: Combine the 4mg palladium nanosheets obtained in step one with 4mg palladium acetylacetonate, 60mg cetyltrimethylammonium bromide, 50mg ascorbic acid and 50mg polyvinylpyrrolidone (M w =30000) was added to 10mL N,N dimethylformamide, stirred for 10min to fully dissolve the palladium acetylaceton...

Example Embodiment

[0047] Example 2

[0048] Step 1. Dissolve 16mg of palladium acetylacetonate, 60mg of cetyltrimethylammonium bromide, 100mg of tungsten carbonyl, 170mg of citric acid and 30mg of polyvinylpyrrolidone in 10mL of N, N dimethylformamide and stir for 1 hour to make each The substance was fully dissolved, and the reaction solution was transferred to a 25 mL round bottom flask, and reacted at 80°C for 1 h. After the reaction is completed, the reaction solution is centrifuged to obtain hexagonal palladium nanosheets. The morphology of the palladium nanosheets is like Figure 5 (a) Shown. The thickness of the hexagonal palladium nanosheets is 1.0 nm, and the average side length is 6.4 nm.

[0049] Step 2: Combine the 4mg palladium nanosheets obtained in step one with 4mg palladium acetylacetonate, 30mg cetyltrimethylammonium bromide, 50mg ascorbic acid and 50mg polyvinylpyrrolidone (M w =30000) was added to 10mL N,N dimethylformamide, stirred for 10min to fully dissolve palladium acetyla...

Example Embodiment

[0050] Example 3

[0051] Step 1. Add 16mg of palladium acetylacetonate, 60mg of cetyltrimethylammonium bromide, 100mg of tungsten carbonyl, 50mg of citric acid and 30mg of polyvinylpyrrolidone into 10mL of N, N dimethylformamide and stir for 1 hour to make each The substance was fully dissolved, and the reaction solution was transferred to a 25 mL round-bottomed flask, and reacted at 80°C for 1 h. After the reaction is completed, the reaction solution is centrifuged to obtain hexagonal palladium nanosheets. The morphology of the palladium nanosheets is like Figure 5 (b) Shown. The thickness of the hexagonal palladium nanosheets is 1.1 nm, and the average side length is 24.5 nm.

[0052] Step 2: Combine the 4mg palladium nanosheets obtained in step one with 4mg palladium acetylacetonate, 120mg cetyltrimethylammonium bromide, 50mg ascorbic acid and 50mg polyvinylpyrrolidone (M w =30000) was added to 10mL N,N dimethylformamide, stirred for 10min to fully dissolve palladium acetyla...

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Abstract

The invention discloses a preparation method of a two-dimensional hollow palladium nanocrystal. A palladium nanoseed, a palladium precursor, a bromide ion modifier, a reductive agent and a dispersing agent are added into solvent for reacting, and accordingly the two-dimensional hollow palladium nanocrystal is prepared, wherein the palladium nanoseed is a palladium nanosheet. According to the preparation method, the nanosheet is used as the seed to be further reacted so that the two-dimensional hollow palladium nanocrystal can be prepared. Operating is easy, the reaction condition is mild, the reagent is low in price, the toxicity is small, and implementation is easy. The invention further discloses the two-dimensional hollow palladium nanocrystal prepared through the preparation method. The upper surface and the lower surface of the two-dimensional hollow palladium nanocrystal are {111} crystal faces, the thickness of the two-dimensional hollow palladium nanocrystal is 2-4 nm, the two-dimensional hollow palladium nanocrystal is of an ultrathin annular structure, the material specific area and the atom utilization rate are improved, and the catalytic performance of the palladium nanocrystal is effectively enhanced.

Description

technical field [0001] The invention relates to the field of preparation of noble metal nanomaterials, in particular to a two-dimensional hollow palladium nanocrystal and a preparation method thereof. Background technique [0002] As an important noble metal nanomaterial, palladium nanocrystals are widely used in the fields of hydrogenation reaction, carbon-carbon coupling and carbon monoxide treatment due to their good catalytic performance and relatively low price. Some research results in recent years have also found that palladium Nanocrystals also have potential applications in areas such as surface plasmon resonance. [0003] Studies have shown that the morphology of palladium nanocrystals has a great influence on their properties. Controlling the morphology of palladium nanocrystals has always been a research hotspot in the industry. At present, many literatures have reported that a variety of nanostructures have been prepared by using thermodynamic control methods. ...

Claims

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Application Information

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IPC IPC(8): B22F9/24B82Y30/00B82Y40/00
Inventor 张辉李毅颜聿聪杨德仁
Owner ZHEJIANG UNIV
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