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A magnetic hollow micro-nano material and its preparation method and application

A micro-nano and micro-nano ball technology, applied in the field of magnetic hollow micro-nano materials and their preparation, and the field of preparing magnetic hollow micro-nano materials, can solve the problems of strict requirements on instrument accuracy, cumbersome steps, long time consumption, etc., to achieve structural and The formation mechanism is novel, the production equipment is simple, and the production cycle is short.

Active Publication Date: 2021-09-21
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although the above-mentioned patent documents mainly use the template-assisted method to prepare magnetic metal nanotubes, the preparation method is highly dependent on the template, the steps are cumbersome, and the accuracy of the instrument is strict and time-consuming, so it is not suitable for industrial production and application.

Method used

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  • A magnetic hollow micro-nano material and its preparation method and application
  • A magnetic hollow micro-nano material and its preparation method and application
  • A magnetic hollow micro-nano material and its preparation method and application

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preparation example Construction

[0048] The invention also discloses a preparation method of magnetic hollow micro-nano material, the specific steps include:

[0049] (1) Dissolving copper salt, nickel salt and ethylenediamine in alkali solution, stirring and reacting at room temperature for 20-40 minutes, to obtain mixture 1;

[0050] (2) Add hydrazine hydrate to mixture 1, feed oxidizing gas at the same time, heat and stir, wait for the reaction to be completed, drop to room temperature, obtain mixture 2;

[0051] (3) The mixture 2 was centrifugally filtered, washed three times, and then dried to finally obtain the magnetic hollow micro-nano material disclosed in the present invention.

[0052] In order to further optimize the above-mentioned technical scheme, in the reaction system of step (1), the ratio of the addition amount of nickel salt to copper salt is (1~20):1, and the concentration of nickel salt is 0.5~8.0mol / L, ethylene two The concentration of amine is 2-8 mol / L.

[0053] In order to further ...

Embodiment 1

[0058] Prepare 900mL of 7.0M NaOH solution in a 1L beaker, cool to room temperature, and then add 7.8mL of 0.5mol / L Cu(NO 3 ) 2 ·3H 2 O, 4.2mL 0.5mol / L Ni(NO 3 ) 2 ·6H 2 O, 9mL ethylenediamine (EDA) was successively added into the beaker, after stirring for 20-40min, 1.5mL hydrazine hydrate (N 2 h 4 ·H 2 O), then stirred for 20 to 40 minutes, passed into an oxidizing gas at 90°C (air flow rate was 20mL / min) and continued to heat and stir (stirring speed 1200 rpm) for 5 hours, took it out and cooled it to room temperature naturally, and used distilled water, Wash each with absolute ethanol 3 times, centrifuge and dry in a vacuum oven at 40°C to obtain magnetic hollow micro-nanotubes.

[0059] The composition, phase, morphology and static magnetic properties of the obtained product measured under energy spectrum, XRD, scanning electron microscope and VSM are as follows: Figure 1~4 shown. It can be seen that the product is a homogeneous and monodisperse hollow micro-nan...

Embodiment 2

[0062] Compared with the preparation steps disclosed in Example 1, the only difference is that the reaction temperature is 80° C., and the rest of the preparation steps and process parameters are the same.

[0063] The composition, phase and morphology of the obtained product measured under energy spectrum, XRD and scanning electron microscope are as follows: Figure 6-8 shown. It can be seen that the product is a homogeneous and monodisperse hollow micro-nanotube. Wherein, the diameter of the hollow micro-nanotube is 490-690 nm, the wall thickness is 25-110 nm, the length is about 3-11 μm, and the atomic ratio of Cu / Ni is 0.00685.

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Abstract

The invention discloses a magnetic hollow micro-nano material, a preparation method and application thereof, and belongs to the technical field of nano-materials. The invention discloses that the magnetic hollow micro-nano material prepared by a one-step liquid-phase reduction-oxidation method not only has a novel structure and formation mechanism, but also can regulate the concentration of Cu and Ni by changing the reaction temperature, time, stirring speed, gas flow, and reactant concentration. Content and composition, morphology and structure of magnetic hollow micro-nano materials, in which the diameter of micro-nanotubes is 0.1-2 μm, the length is 2-12 μm, and the wall thickness is 10-140 nm; the diameter of micro-nanospheres is 0.2-5 μm, and the wall thickness is 10~180nm. Because of the good dispersion and uniformity of the magnetic hollow micro-nano material and good microwave absorption characteristics, it is widely used in the fields of microwave absorption and shielding, electrocatalysis, lithium-ion batteries, and surface-enhanced Raman spectroscopy. In addition, the preparation method disclosed in the present invention is simple to operate, environmentally friendly, has good potential for industrial application, and is suitable for market promotion and application.

Description

technical field [0001] The invention belongs to the technical field of nanometer materials, and relates to a simple method for preparing magnetic hollow micronanomaterials. More specifically, it relates to a magnetic hollow micro-nano material and its preparation method and application. Background technique [0002] In recent years, magnetic metal and alloy nanomaterials have been widely used in ultra-high density information storage, catalysis, giant magnetoresistance, magneto-optic materials, microwave absorbing materials, ferrofluids and biomedicine due to their excellent electrical, magnetic and catalytic properties. etc. have shown great application prospects. [0003] Since morphology is an important factor determining performance, hollow nanomaterials are widely used in nano-devices, sensors, energy, Storage and energy conversion and other fields have important application prospects. At present, the main technologies for preparing magnetic metal nanotubes include e...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F1/00B22F9/24H01F1/01H01F41/00B01J23/755C09K3/00
CPCB22F9/24H01F1/01H01F41/00B01J23/755B01J35/0033C09K3/00B22F1/0549B22F1/0655B22F1/0547
Inventor 童国秀刘敏敏陈悦刘妤吴文华
Owner ZHEJIANG NORMAL UNIVERSITY
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