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Magnetic alloy hollow microsphere and preparation method thereof

A magnetic alloy and microsphere technology, applied in the nanometer field, can solve the problems of high temperature energy consumption, complicated and multi-step, harsh conditions, etc., and achieve the effect of no template, cheap raw materials, and short time

Active Publication Date: 2018-09-14
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above method adopts hard template, high temperature calcination or electroless plating process, so there are disadvantages such as complicated and multi-step, high temperature energy consumption, special requirements for equipment, long cycle and harsh conditions.

Method used

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  • Magnetic alloy hollow microsphere and preparation method thereof
  • Magnetic alloy hollow microsphere and preparation method thereof
  • Magnetic alloy hollow microsphere and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Dissolve 1.2g (12g / L) surfactant [polyvinylpyrrolidone (PVP)] in a mixed solution of 98mL pure ethylene glycol and 4.5mL deionized water and stir evenly, then add 0.6424g (0.027M) CoCl 2 ·6H 2 O and 0.4279g (0.018M) NiCl 2 ·6H 2 O electric power was stirred for 2 h, and then 2.5 mL of anhydrous hydrazine hydrate was added dropwise to the solution and stirred for 1 h. Then the mixture was heated to 197°C to boil, condensed and refluxed for four hours. After cooling, it was washed with absolute ethanol for multiple times of magnetic separation and separation until the solution was clear, and finally dried to obtain the required magnetic alloy hollow microspheres.

[0034] The phase, elemental composition and morphology of the obtained product observed under the scanning electron microscope are as follows: Figure 1~3 As shown, the particle diameter is 0.72~1.68μm, and the wall thickness is 28~73nm; figure 2 As shown, the Co / Ni atomic ratio is 1.96; the static magneti...

Embodiment 2

[0036] Same step as Example 1, but only add 1.0706g (0.045M) CoCl in the solution 2 ·6H 2 O, the morphology of the resulting product observed under the scanning electron microscope is as follows Figure 8As shown, the particle diameter is 0.84-1.85 μm, and the wall thickness is 4-17 nm. Static magnetic properties such as Figure 5 , the saturation magnetization is 152.89emu·g -1 ; Its two-dimensional reflectivity is as follows Figure 9 As shown, paraffin is used as the base, when the mass fraction is 50%, the reflectance is -18.08dB at 2GHz, and the sample thickness is 7.9mm.

Embodiment 3

[0038] Same as Example 1, but add 0.5353g (0.0225M) CoCl to the solution simultaneously 2 ·6H 2 O and 0.5348g (0.0225M) NiCl 2 ·6H 2 O. The morphology of the obtained product observed under the scanning electron microscope is as follows: Figure 10 As shown, the particle diameter is 0.76-1.82 μm, and the wall thickness is 47-78 nm. Energy spectrum analysis such as figure 2 As shown, the Co / Ni atomic ratio is 1.69. Static magnetic properties such as Figure 5 , the saturation magnetization is 105.93emu g -1 ; its electromagnetic parameters such as Figure 5-6 As shown, in the frequency range of 2-18GHz, the real part and imaginary part of the permittivity increase by 0.75-1.39 and 0.21-0.79 times respectively compared with the hollow Co sphere, and the real part and imaginary part of the permeability increase by 0.98-1.02 compared with the and 0.11 to 0.96 times. Its two-dimensional reflectivity is as Figure 11 As shown, paraffin is used as the base, when the mass ...

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Abstract

The invention provides a magnetic alloy hollow microsphere and a preparation method thereof. The components of the microsphere comprise cobalt and nickel. The structural formula of the microsphere isshown as Capable of<x>Ni<1-x>, wherein x is greater than or equal to 0.14 and less than or equal to 1. The microsphere is of a hollow structure and has the diameter being 0.32-3.35 microns, the wall thickness being 4-370 nm and the saturation magnetization intensity being 80.4-152.89 emu.g<-1>. The microsphere is prepared through a mixed solvent high-temperature liquid phase reduction method. Thepreparation method comprises the steps of adding an organic solvent, water and a surface active agent into three flasks in proportion to be stirred for 10 min; adding metal salt to be subjected to electric stirring for 2 h, and dropwise adding a reducing agent to be subjected to electric stirring for 1 h; conducting reflux condensation at 170-197 DEG C for 3-4 h, and conducting repeated magnetic separating and washing through ethanol after cooling; and finally, conducting drying to obtain the required magnetic alloy hollow microsphere. The magnetic alloy hollow microsphere is made of a raw material which is low in price and easy to get. The magnetic alloy hollow microsphere is low in cost, simple in process, high in efficiency and easy to popularize. A magnetic ball chain has the properties of size and composition adjustability and can be applied to magneto-rheological, magnetic separation, catalytic and electrode materials and microwave absorption or high-density magnetic recording materials.

Description

technical field [0001] The invention relates to the field of nanotechnology, in particular to a simple method for preparing magnetic alloy hollow microspheres. Background technique [0002] Due to their unique electrical, optical, magnetic and excellent chemical properties, magnetic metal nanomaterials have been widely used in nuclear magnetic resonance imaging, optical nanodevices, targeted drugs, magnetic storage, catalysts, etc. Among them, hollow magnetic micro-nano materials have attracted much attention because of their low density, high specific surface area, low thermal expansion coefficient and refractive index. The methods for preparing hollow microspheres mainly include traditional hard template method, sacrificial template synthesis method, soft template preparation method and template-free method. At present, only a few literatures and patents report the preparation of magnetic metal / alloy hollow microspheres. Chinese patent document (CN201510083390.8) disclos...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B22F9/24B22F1/00B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00B22F9/24B22F1/0549B22F1/0655B22F1/07B22F1/054
Inventor 童国秀刘琳孙嘉诚乔儒陈锦绣宫培军韩佳女胡潘冰吴文华
Owner ZHEJIANG NORMAL UNIVERSITY
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