One-step microwave preparation method for bimetal/carbon layered composite sphere

A technology of bimetal and composite balls, applied in the field of preparation of bimetal/carbon composite balls, can solve the problems of complicated steps and non-uniform products, and achieve the effects of good monodispersity, good controllability and high yield

Active Publication Date: 2014-02-19
NANJING UNIV +1
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

The doping of two kinds of metal particles can be achieved by using a two-step method (that is, obtaining composite spheres of carbon-coated metal nanoparticles first, and then depositing a second metal on the surface of the spheres), but the steps are cumbersome, the products are no

Method used

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  • One-step microwave preparation method for bimetal/carbon layered composite sphere
  • One-step microwave preparation method for bimetal/carbon layered composite sphere
  • One-step microwave preparation method for bimetal/carbon layered composite sphere

Examples

Experimental program
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Effect test

Embodiment 1

[0035] Preparation of palladium nanoparticles-doped carbon (Pd / C) composite spheres: Add 0.1 g of dry microporous carbon spheres to 50 mL of PdCl at a concentration of 2 mM at room temperature 2 solution for immersion. After soaking for 0.5h, add 0.05g polyvinylpyrrolidone and stir vigorously until completely dissolved. Then, the carbon sphere suspension was placed in a microwave reactor and reacted for 10 min under the condition of microwave power of 140W. After the reaction vessel was taken out, it was naturally cooled to room temperature in the air, washed repeatedly by centrifugation with deionized water and absolute ethanol, and finally dried in an oven or dried for more than 6 hours.

Embodiment 2

[0037] Change the K of the precursor to 2 mM 2 PdCl 4 Solution, other conditions are with embodiment 1.

Embodiment 3

[0039] Change the heating condition to 100° C. water bath for 6 hours, and the other conditions are the same as in Example 1.

[0040] figure 1 It is the TEM picture of the product obtained when the same concentration, immersion time, microwave power and reaction time are used, but the palladium solution precursor is different. from figure 1 a It can be seen that the product obtained in Example 1 is a composite sphere uniformly doped with nanoparticles. TEM of a single composite sphere ( figure 1 b) shows that a large number of nanoparticles (8–10 nm in size) are located inside the carbon sphere, while there are almost no particles on the surface of the sphere. The SEM image (figure omitted) also confirms that there are no nanoparticles on the surface of the carbon spheres. The number density of nanoparticles in the area close to the surface of the sphere is higher than that in the central area, indicating that they are distributed in a spherical shell with a certain thick...

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Abstract

The invention discloses a bimetal/carbon layered composite sphere and a simple and quick preparation method for the same. The preparation method is based on merits of microwave heating, and includes that mixed liquor containing metal ions {including positive ions such as [Ag(NH<3>)<2>]<+>, Pd<2+> and Au<+> and negative ions such as MCl<n>(wherein the M represents Au, Pd and Pt)} with different electric charges is used as a precursor, and different types of metal selectively are grown inside and outside a carbon sphere simultaneously, so that the bimetal carbon-doped layered composite sphere with nano-particles can be prepared. The bimetal/carbon layered composite sphere and the preparation method have the advantages that an integral preparation procedure only takes 2-10 minutes, and reaction parameters are adjusted, so that the sizes, the number density and the positions of the metal nano-particles can be controlled; the shortcoming of difficulty in growing more than two types of metal nano-particles inside a preliminarily prepared carbon sphere can be overcome, and the constraint that usually only alloy can be generated via co-reduction of mixed metal ions under the condition of traditional heating is broken through; devices applied in the preparation method are simple, operation is easy, the controllability is good, and the preparation method can be particularly popularized to controllable preparation for other bimetal doped multilayer composite materials with nano-particles.

Description

technical field [0001] The invention relates to bimetallic / carbon layered composite spheres used in the fields of optics, catalysis, and biosensing, and a simple and fast preparation method thereof, in particular to the realization of two metals or metal complex ions with different charges on carbon by one-step microwave The interior and the surface are simultaneously reduced to obtain a bimetal / carbon composite sphere with a layered structure. Background technique [0002] Doping metal nanoparticles into the interior or surface of the spherical matrix can obtain catalytic, magnetic, electrical, optical and other properties different from metal nanoparticles and their random aggregates. The small size effect, collective effect, and metal-matrix synergy of nanoparticles have important effects on the performance improvement. Especially in the aspect of catalysis, the micropores of the matrix material have a confinement effect on the nanoparticles, which can enhance the cataly...

Claims

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Application Information

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IPC IPC(8): B22F9/24
Inventor 唐少春孟祥康李楠庭高文华
Owner NANJING UNIV
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