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Graphene-coated magnetic nickel nanoparticle 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: 2014-10-15
SHENZHEN EIGEN EQUATION GRAPHENE TECH CO LTD
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  • Summary
  • 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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  • Graphene-coated magnetic nickel nanoparticle and preparation method thereof
  • Graphene-coated magnetic nickel nanoparticle and preparation method thereof
  • Graphene-coated magnetic nickel nanoparticle and preparation method thereof

Examples

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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 nickel oxide, 20ml 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 get the pre-oxidized Body (i.e. 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 diffraction analysis spectr...

Embodiment 2

[0058] Stir 7.5g of LPAN solution (molecular weight 1600) at 100°C for 200h to form a microcyclized LPAN solution, and heat-treat the microcyclized LPAN solution at 300°C for 1h to form a thermally oxidized polyacrylonitrile with a ladder structure. Polymer (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 obtain thermal oxidation Prebody. 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, 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 of nickel oxide, 15ml 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 get the pre-oxidized Body (i.e. 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 metal particles, ...

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Abstract

The invention discloses a graphene-coated magnetic nickel nanoparticle and a preparation method thereof. The method includes the following steps: thermally oxidated polyacrylonitrile oligomer and nickel compound are added into solvent and mixed uniformly, so that LPAN-coated nickel compound is obtained; the uniformly mixed LPAN-coated nickel compound is dried under 200 DEG C to 250 DEG C for 1 to 10 hours until the solvent is evaporated completely, so that low-temperature carbonized precursor-coated nickel compound is obtained; the low-temperature carbonized precursor-coated nickel compound is calcined for 1 to 10 hours under inert gas shielding and the conditions of gas flow ranging from 10ml / min to 500ml / min and 700 DEG C to 1500 DEG C, and thereby the graphene-coated magnetic nickel nanoparticle is obtained. The preparation method has the advantages of simple equipment and process, low cost, high purity, high output, uniform particle size distribution, good morphology 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 Applications(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