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Metallic nano cluster/silicon dioxide hollow nuclear shell structured nanoparticles and preparation method thereof

A metal nanocluster and core-shell structure technology, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of limiting the application performance of hollow metals with nanostructures, and the inability to control and adjust synchronously, so as to achieve controllable size and shape, Easy to operate, high output effect

Active Publication Date: 2011-04-20
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although the above method can be made of nanostructured solid metal @SiO 2 Get Nanostructured Hollow Metal@SiO 2 , but the metal coated in the silica shell is only nanoparticles, not metal nanoclusters; at the same time, the shape and size of the cavity depend on the pre-synthesized nanostructured solid metal@SiO 2 The shape and size of the cavity, the cavity shape, the cavity size, and the thickness of the shell cannot be adjusted synchronously, which greatly limits the nanostructured hollow metal @SiO 2 application performance

Method used

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  • Metallic nano cluster/silicon dioxide hollow nuclear shell structured nanoparticles and preparation method thereof
  • Metallic nano cluster/silicon dioxide hollow nuclear shell structured nanoparticles and preparation method thereof
  • Metallic nano cluster/silicon dioxide hollow nuclear shell structured nanoparticles and preparation method thereof

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Embodiment 1

[0046] 10g Dissolve in 50mL cyclohexane, stir and heat to 50°C, after complete dissolution, add 1.5mL of 1M cobalt chloride solution dropwise, stir for 1h, add 2mL of 80% hydrazine hydrate solution, stir for 5-50 minutes, adjust the reaction with ammonia water The pH value of the solution is 10.5-11, 10 g of ethyl orthosilicate is added dropwise, and the reaction is stirred for 2 hours. After centrifugation, washing, drying, roasting, and reduction, electron microscope observation is carried out, such as figure 1 As shown, the product particles are uniform, the particle size is 40-50nm, the nano-metal particle size is <4nm, and the cavity diameter is 8-10nm.

Embodiment 2

[0048] 10g Dissolve in 50mL cyclohexane, stir and heat to 50°C, after complete dissolution, add 1.5mL 1M cobalt chloride solution dropwise, stir for 1h, then add 1.5mL 1M ethylenediamine (or triethanolamine / diethylenetriamine / tetra ethylenepentamine) solution, after being uniformly dispersed, add 1.0 g of NaBH 4 / LiAlH 4 , stirred and reacted for 5-50 minutes, adjusted the pH value of the reaction solution to 10.5-11 with ammonia water, added 10 g of ethyl orthosilicate dropwise, and stirred and reacted for 2 hours. After centrifugation, washing, drying, roasting, and reduction, electron microscope observation is carried out, such as figure 2 As shown, the product particles are uniform, the particle size is 40-50nm, the nano-metal particle size is <4nm, and the cavity diameter is 8-10nm.

Embodiment 3

[0050] 10g Dissolve in 50mL cyclohexane, stir and heat to 50°C, after complete dissolution, add 1.5mL of 1M nickel nitrate solution dropwise, stir for 1h, add 2mL of 80% hydrazine hydrate solution, stir for 5-50 minutes, adjust the reaction solution with ammonia water The pH value is 10.5-11, 10 g of ethyl orthosilicate is added dropwise, and the reaction is stirred for 2 hours. After centrifugation, washing, drying, roasting, and reduction, electron microscope observation is carried out, such as image 3 As shown, the product particles are uniform, the particle size is 20-30nm, the nano-metal particle size is <4nm, and the cavity diameter is 8-10nm.

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Abstract

The invention belongs to the field of nanoparticle preparation, in particular to metallic nano cluster / silicon dioxide hollow nuclear shell structured nanoparticles and a one-step controllable preparation method thereof. The used surfactant is a nonionic surfactant, the organic phase is cyclohexane, toluene and other organic hydrocarbons, and a metal saline solution and a metal complexing agent are added to form a reversed micelle system. Meanwhile, the complexed metal saline solution in the reversed micelle system is reduced to obtain metallic nanoparticles and then ammonia water and ammoniawater are added directly in the solution to obtain size and shape controllable hollow silicon dioxide nuclear shell material with metallic nano clusters distributed uniformly on the inner wall of thecavity. The method has the advantages of simple process, easy operation and great yield and can obtain size and shape controllable metallic nano cluster / silicon dioxide hollow nuclear shell structured nanoparticles.

Description

technical field [0001] The invention belongs to the field of nanoparticle preparation, and in particular relates to a metal nanocluster@silica hollow core-shell nanoparticle and a one-step controllable preparation method thereof. Background technique [0002] Nano-sized core-shell materials have great application potential in chemistry, physics, electronics, biotechnology, and material science, and have received extensive attention. The hollow core-shell material has low density, high surface area, good thermal and mechanical stability, especially the nano-sized hollow metal core-silica shell material with controllable structure, composition and performance in catalytic nanoreactors, sensors. And energy storage media and other aspects have shown outstanding advantages, so it has become a hot spot of interdisciplinary research. [0003] Synthesis of nanostructured metal@SiO by conventional methods 2 Only solid structures can be obtained. At present, nanostructured hollow me...

Claims

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Application Information

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IPC IPC(8): B22F9/24B22F1/02B01J13/02
Inventor 吕荣文邹伟
Owner DALIAN UNIV OF TECH
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