Fe/(SiO-[2]ú½C) core-shell composite nanometer particle with high stability and method for preparing same

A composite nanoparticle, composite nanoparticle technology, applied in nanostructure manufacturing, inductor/transformer/magnet manufacturing, nanotechnology, etc., can solve problems such as hindering the application process of iron nanoparticles, unsuitable for large-scale production, and cumbersome preparation process. , to achieve the effect of improved resistivity, high product stability and simple preparation process

Inactive Publication Date: 2005-06-29
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, nano-sized transition metals are very easy to oxidize in air and even spontaneously ignite at room temperature, which seriously hinders the practical application of iron nanoparticles.
At present, iron nanoparticles are generally prepared in vacuum (less than 10 -6 Pa) or in inert gases such as argon and helium at low pressure, the preparation process is loaded down with trivial details, equipment requirements are high, and it is not suitable for large-scale production

Method used

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  • Fe/(SiO-[2]ú½C) core-shell composite nanometer particle with high stability and method for preparing same
  • Fe/(SiO-[2]ú½C) core-shell composite nanometer particle with high stability and method for preparing same
  • Fe/(SiO-[2]ú½C) core-shell composite nanometer particle with high stability and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: Under strong stirring, dissolve 0.01mol ferric chloride and 0.015mol citric acid in 100mL of absolute ethanol, and continue stirring at 60°C for 6 hours to form a uniform transparent sol; add 0.1mL ethyl orthosilicate, 80 °C to evaporate and dehydrate until the xerogel is formed; the xerogel was pre-calcined at 450 °C in air for 3 hours, and then placed in a tube furnace for reduction at 800 °C for 4 hours in a hydrogen atmosphere. Hydrocarbon gas was then introduced at 600°C for 0.1 hour. The resulting product is an amorphous SiO 2 and carbon shell, the core is cubic α-Fe and a large amount of Fe 3 Composite nanoparticles of C. The resulting product is an amorphous SiO 2 The shell, the core is a composite nanoparticle of α-Fe in the cubic crystal phase, the magnetic measurement results are shown in figure 2, Saturation magnetization 193.61Am 2 / kg.

[0015] Use FeCl 2 4H 2 O, ferric nitrate obtains the similar result with above-mentioned.

[0016] ...

Embodiment 2

[0017] Example 2: under strong stirring, 0.01mol FeCl 2 4H 2 O and 0.015mol citric acid were dissolved in 100mL of absolute ethanol, and stirred continuously at 60°C for 6 hours to form a uniform transparent sol; add 0.1mL tetraethyl orthosilicate, and evaporate and concentrate at 80°C until a dry gel was formed; the dry gel was dried in air Pre-calcined at 450°C for 3 hours, then placed in a tube furnace for hydrogen reduction at 800°C for 4 hours, and then passed through methane, ethane or butane, ethylene, acetylene, etc. at 400°C for 0.5 hours. Hydrocarbon gases are not significantly different. The resulting product is an amorphous SiO 2 and carbon shell, the core is cubic α-Fe and a large amount of Fe 3 Composite nanoparticles of C. For magnetic measurements see figure 2, Saturation magnetization 76.53Am 2 / kg.

Embodiment 3

[0018] Example 3: under strong stirring, 0.01mol FeCl 2 4H 2 O and 0.015mol citric acid were dissolved in 100mL of absolute ethanol, and stirred continuously at 60°C for 6 hours to form a uniform transparent sol; add 0.1mL tetraethyl orthosilicate, and evaporate and concentrate at 80°C until a dry gel was formed; the dry gel was dried in air Pre-calcined at 450°C for 3 hours, then placed in a tube furnace in a hydrogen atmosphere for reduction at 800°C for 4 hours, then passed through methane, ethane or butane, ethylene, acetylene, etc. at 400°C for 0.5 hours, and finally in argon Incubate at 750°C for four hours in atmosphere. The resulting product is an amorphous SiO 2 and carbon shell, the core is a composite nanoparticle of α-Fe in the cubic crystal phase, and a very small amount of Fe 3 c. For magnetic measurements see figure 2, Saturation magnetization 116Am 2 / kg. Magnetic measurements of Comparative Example 2 show that after annealing in argon, more Fe 3 C is ...

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Abstract

It is a compound nanometer particles of Fe / (SiO#-[2]+C) nucleus or shell with high stability. The process method comprises the following steps: to use iron salt as material and citric acid or other organic acid and organic amine as bonding agent and non-water ethanol as solve agent to form even non-water glue; to join silicic acid ethyl acetate and after vaporizing and condense to form solid glue; to pre-sinter in the air to remove the organic material; to deoxidize in H#-[2] and different temperatures to get the particles.

Description

1. Technical field [0001] The present invention relates to a kind of Fe / (SiO with core / shell structure, high magnetization, high stability 2 +C) Composite nanoparticles and preparation methods thereof. 2. Background technology [0002] Iron is a metal with the largest magnetic moment among the magnetic transition elements. Iron nanoparticle made of metal iron has the characteristics of quantum size effect, small size effect, surface effect, etc., and thus exhibits many unique properties. It has broad application prospects. The research on the preparation and properties of iron nanoparticles has aroused widespread interest. However, nano-sized transition metals are very easy to oxidize in air and even spontaneously ignite at room temperature, which seriously hinders the practical application of iron nanoparticles. At present, iron nanoparticles are generally prepared in vacuum (less than 10 -6 Pa) or in inert gases such as argon and helium at low pressure, the preparatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B82B1/00B82B3/00H01F1/01H01F41/02
Inventor 汤怒江钟伟都有为
Owner NANJING UNIV
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