A kind of graphene-coated magnetic nano-nickel particles and preparation method thereof

A graphene-coated, magnetic nanotechnology, applied in the direction of the magnetism of inorganic materials, can solve the problems of easy oxidation of metal nanoparticles, low saturation magnetization, complex process, etc., and achieve high magnetic saturation value, good shape, and equipment technology. simple effect

Active Publication Date: 2016-06-29
SHENZHEN EIGEN EQUATION GRAPHENE TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In view of the above deficiencies in the prior art, the object of the present invention is to provide a graphene-coated magnetic nano-nickel particle and a preparation method thereof, aiming at solving the problem of low yield, complex process, low saturation magnetization and metal nano-nickel particles in the existing preparation method. Particles are easy to oxidize, etc.

Method used

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  • A kind of graphene-coated magnetic nano-nickel particles and preparation method thereof
  • A kind of graphene-coated magnetic nano-nickel particles and preparation method thereof
  • A kind of graphene-coated magnetic nano-nickel particles and preparation method thereof

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Embodiment 1

[0056] Stir 3g of LPAN solution (molecular weight 4000) at 120°C for 120h to form a microcyclized LPAN solution, heat-treat the microcyclized LPAN solution at 250°C for 8h to form a thermally oxidized polyacrylonitrile oligomer with a ladder structure (OPAN) solid, add 7.6g of nickel oxide, 20ml of solvent, and ball mill the sample with a planetary ball mill, the ball to material ratio is 7:1, 500rad / min ball mill for 10h, after discharging, dry in an oven at 230°C for 3h to obtain the thermal oxidation precursor (That is, low temperature carbonization precursor coated nickel compound). Put the thermal oxidation precursor in a porcelain boat, under the protection of an inert atmosphere, with a gas flow rate of 150ml / min, calcinate at 900°C for 4 hours, and cool to room temperature to obtain a graphene-coated nickel magnetic nanoparticle composite. The product structure is as follows: Figure 2a (SEM spectrum, scanning electron microscope spectrum), 2b (XRD spectrum, X-ray diff...

Embodiment ２

[0058] Stir 7.5g of LPAN solution (molecular weight 1600) at 100°C for 200h to form a microcyclized LPAN solution, heat-treat the microcyclized LPAN solution at 300°C for 1h to form a thermally oxidized polyacrylonitrile oligomer with a ladder structure (OPAN) solid, add 3.17g nickel oxide, 30ml solvent, and ball mill the sample with a planetary ball mill, the ball to material ratio is 7:1, 500rad / min ball mill for 10h, after discharging, dry in an oven at 230°C for 10h to get the pre-oxidized body. Put the thermal oxidation precursor in a porcelain boat, under the protection of an inert atmosphere, with a gas flow rate of 150ml / min, calcined at 1300°C for 4 hours, and cooled to room temperature to obtain a composite of graphene-coated nickel magnetic nanoparticles. The product structure is as follows: Figure 3a (SEM spectrum, scanning electron microscope spectrum), 3b (XRD spectrum, X-ray diffraction analysis spectrum).

Embodiment 3

[0060] Stir 3g of LPAN solution (molecular weight: 25,000) at 200°C for 100h to form a microcyclized LPAN solution, then heat-treat the microcyclized LPAN solution at 200°C for 10h to form a thermally oxidized polyacrylonitrile oligomer with a ladder structure (OPAN) solid, add 7.6g nickel oxide, 15ml solvent, and ball mill the sample with a planetary ball mill, the ball to material ratio is 7:1, 500rad / min ball mill for 10h, after discharging, dry in an oven at 230°C for 3h to obtain the thermal oxidation precursor (That is, low temperature carbonization precursor coated nickel compound). The thermal oxidation precursor was placed in a porcelain boat, under the protection of an inert atmosphere, the gas flow rate was 150ml / min, calcined at 700°C for 4h, and cooled to room temperature to obtain a graphene-coated nickel magnetic nanoparticle composite.

[0061] Compared with the traditional synthesis method, the present invention adopts the production method of graphene-coated ...

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Abstract

The invention discloses a graphene-coated magnetic nano-nickel particle and a preparation method thereof. The method comprises the following steps: adding thermally oxidized polyacrylonitrile oligomers and nickel compounds into a solvent, and mixing them uniformly to obtain LPAN-coated nickel Compound; dry the mixed LPAN-coated nickel compound at 200°C-250°C for 1-10h until the solvent is completely evaporated to obtain a low-temperature carbonization precursor-coated nickel compound. The low-temperature carbonization precursor-coated nickel compound is calcined for 1-10 hours at a gas flow rate of 10-500ml / min and 700-1500°C under the protection of an inert atmosphere to obtain graphene-coated magnetic nano-nickel particles. The preparation method of the invention has the advantages of simple equipment and process, low cost, high purity, large output, uniform particle size distribution, good appearance and the like.

Description

technical field [0001] The invention relates to the field of novel magnetic nanometer materials, in particular to a graphene-coated magnetic nanometer nickel particle and a preparation method thereof. Background technique [0002] Magnetic nanoparticles have a wide range of applications, including magnetic fluids, catalysts, biotechnology, biomedicine, nuclear magnetic resonance imaging, data storage, and environmental remediation, and thus have aroused great interest among researchers. In most envisaged applications of magnetic nanoparticles, the performance of the particles is best when the size is smaller than a critical value. Different materials have different particle sizes, but most of them are between 10 and 20nm. [0003] However, in this size range, storage of nanoparticles for too long can lead to inherent instability problems in nanomaterials. Such small particles, due to their large surface area and high volume ratio, tend to reduce their surface energy and ten...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F1/02H01F1/01
Inventor 刘剑洪张黔玲何传新徐坚廖楚宏任响宁李晓明
Owner SHENZHEN EIGEN EQUATION GRAPHENE TECH CO LTD
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