CN105935777A - Method for preparing graphene/nano nickel composite material - Google Patents

Method for preparing graphene/nano nickel composite material Download PDF

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Publication number
CN105935777A
CN105935777A CN201610266045.2A CN201610266045A CN105935777A CN 105935777 A CN105935777 A CN 105935777A CN 201610266045 A CN201610266045 A CN 201610266045A CN 105935777 A CN105935777 A CN 105935777A
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composite material
nickel composite
graphene
preparing graphene
method preparing
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CN201610266045.2A
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CN105935777B (en
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李天军
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University of Shaoxing
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University of Shaoxing
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM

Abstract

The invention relates to a method for preparing a graphene/nano nickel composite material. The method comprises the following steps: 1) mixing glucose and nickel nitrate, and then grinding through an agate mortar; 2) mixing sodium chloride and potassium chloride, and performing ball milling through a ball mill; 3) uniformly mixing the materials obtained in step 1) and step 2), and preheating; 4) placing the preheated mixed material into a quadrate porcelain boat shaped vessel, transferring the porcelain boat shaped vessel into a tubular furnace, charging inert gas for protecting, and then roasting at a certain heating rate; 5) maintaining the temperature after roasting; 6) naturally cooling under the inert gas protection until the room temperature is met, and then moving out a sample; and 7) washing the obtained mixture through deionized water, and performing vacuum filtration to obtain the graphene/nano nickel composite material. According to the method, the graphene/nano nickel composite material can be prepared by a one-step synthesis method; glucose is the main raw material of the graphene/nano nickel composite material, so that the graphene/nano nickel composite material has the characteristics of being low in cost, and enabling mass application; and the graphene/nano nickel composite material is a novel electromagnetic wave absorbing material.

Description

A kind of method preparing graphene/nanometer nickel composite material
[technical field]
The present invention relates to the preparation method of a kind of composite, be specifically related to a kind of graphene/nanometer nickel composite material prepared Method, belongs to technical field of nano material.
[background technology]
Along with the fast development of electromagnetic wave technology, except bringing easily simultaneously, also bring bigger electromagnetic radiation Polluting, anti-electromagnetic radiation the most slowly develops into a new subject, increasingly obtains the attention of people, and research and development are to electromagnetism wave height The new material of absorbance is expected to solve this problem.Traditional absorbing material is with ferrite as main representative, because it has excellent Good flux loss performance, along with improving constantly that science and technology and people live, the absorbing property of Single Iron ferrite has been got over More can not meet needs, the composite wave-suction material of Development of Novel is a trend, research and development gentlier, thinner, wider, higher new Type absorbing material is current scientific worker's target.
Graphene is a kind of to have excellent mechanics, the material of electricity, both thermally and chemically performance, deposits at photoelectric display, energy The fields such as storage have important application, graphene film edge to have abundant functional group, it is possible to introduce defect polarization and electronics relaxes Polarizing in Henan, is the absorbing material of a kind of excellence.Graphene and metal, metal-oxide, nonmetal oxide and macromolecule material The composite material exhibits of material goes out the electro-magnetic wave absorption ability of excellence, particularly compound, because of the Graphene suction to ripple with metallic nickel Receipts are usually located at high frequency region, and the absorption bands of electromagnetic wave can effectively be widened by graphene/nickel composite.Graphene/nickel is combined Material is possible not only to be greatly improved the loss of electromagnetic wave, is also beneficial to the impedance matching of composite, and the existence of nickel particles also has Help prevent Graphene from reuniting because of Van der Waals adsorption power, form stable three dimensional structure.
And at present the synthetic method of graphene/nanometer nickel composite material is first aoxidized stone with the synthesis of Hummers method mostly Ink alkene (GO), then graphite oxide is reduced to Graphene (RGO), by methods such as hydro-thermals, metallic Ni particles is loaded to Graphene In lamellar structure, complex steps and yield are relatively low, are unsuitable for the large-scale application of this material.
Therefore, for solve above-mentioned technical problem, a kind of innovation of necessary offer prepare graphene/nanometer nickel composite wood The method of material, to overcome described defect of the prior art.
[summary of the invention]
For solving the problems referred to above, it is an object of the invention to provide a kind of extensive, low cost and prepare graphene/nanometer nickel and be combined The method of material.
For achieving the above object, the technical scheme that the present invention takes is: a kind of prepare graphene/nanometer nickel composite material Method, it uses one-step synthesis, comprises the technical steps that:
1), glucose and nickel nitrate are mixed, grinds in agate mortar;
2), sodium chloride and potassium chloride are mixed, through ball mill ball milling;
3), by step 1) and 2) in the material mixing that obtains uniform, and the pre-heat treatment;
4), the mixing material after the pre-heat treatment is placed in square porcelain boat, porcelain boat is positioned over the centre position of tube furnace, is passed through Inert gas shielding, calcines under certain heating rate;
5), isothermal holding is carried out after calcining;
6), under inert gas shielding, it is naturally cooling to room temperature, takes out sample;
7), gained mixture deionized water is cleaned, and obtains product by vacuum filtration.
The method preparing graphene/nanometer nickel composite material of the present invention is further: in step 1), described glucose and The mass ratio of nickel nitrate is (1-16): 1.
The method preparing graphene/nanometer nickel composite material of the present invention is further: step 2) in, described sodium chloride and The mass ratio of potassium chloride is (1-3): 1.
The method preparing graphene/nanometer nickel composite material of the present invention is further: in step 3), the temperature of the pre-heat treatment Degree is 80 DEG C-200 DEG C.
The method preparing graphene/nanometer nickel composite material of the present invention is further: in step 4), and heating rate is 5 DEG C-30 DEG C/min;Calcining heat is 950 DEG C-1300 DEG C;Described noble gas is nitrogen.
The method preparing graphene/nanometer nickel composite material of the present invention is further: in step 5), described temperature retention time For 30min-60min.
The method preparing graphene/nanometer nickel composite material of the present invention is further: in step 6), described dilute hydrochloric acid Concentration is 0.5%.
The method preparing graphene/nanometer nickel composite material of the present invention is further: in step 1), glucose and nitric acid Needing in the mixture of nickel to add ammonium chloride, the mass ratio of described glucose and ammonium chloride is 4:5.
The method preparing graphene/nanometer nickel composite material of the present invention is also: in step 1), glucose 0.1g, nitric acid Nickel 0.1g, grinds 50min;Step 2) in, sodium chloride 11.4g and potassium chloride 2.8g, grinds 50min;In step 3), at 150 DEG C The pre-heat treatment 20h;In step 4), being warming up to 1000 DEG C, heating rate is 20 DEG C/min, is incubated 40min.
Compared with prior art, there is advantages that the present invention can be by the method system of one-step synthesis Standby graphene/nanometer nickel composite material, primary raw material is glucose, therefore have low cost, can the feature of large-scale application, be A kind of novel electromagnetic wave absorbent material.
[accompanying drawing explanation]
Fig. 1 is the X ray diffracting spectrum (XRD) of gained sample of the present invention.
Fig. 2 is field emission scanning electron microscope (SEM) figure of gained sample of the present invention.
[detailed description of the invention]
Embodiment 1:
One, raw material is prefabricated
Weigh 0.8g glucose, 0.05g nickel nitrate, after being sufficiently mixed in glove box, be placed in agate mortar grinding 30min, Obtain mixture A;Weigh 11.5g sodium chloride and 11.5g potassium chloride, to be placed in grinding in ball grinder 30min after being sufficiently mixed, To mixture B;Being mixed by mixture A and B, be placed in square porcelain boat, total mixture amount is less than 2/3rds of porcelain boat total amount.
Two, pretreatment
The mixture of gained in step one is placed in vacuum drying oven, at 80 DEG C of heat treatments 10;
Three, solid state reaction
Gained mixture in step 2 is placed in the middle of tube furnace boiler tube, is passed through nitrogen protection, is warming up to 950 DEG C, heating rate It is 5 DEG C/min, after reaching target temperature, is incubated 30min, naturally cools to room temperature, take out.
Four, product washing
Porcelain boat product in step 3 is taken out, is placed in 500ml beaker, add deionized water, excusing from death stirring 30min, use The filter membrane of 0.5M carries out vacuum filtration, again adds deionized water, repeated washing step, altogether washing 3-5 time.Products therefrom is placed in Air dry oven is dried 24h.
Embodiment 2:
One, raw material is prefabricated
Weigh 0.1g glucose, 0.1g nickel nitrate, after being sufficiently mixed in glove box, be placed in agate mortar grinding 50min, To mixture A;Weigh 11.4g sodium chloride and 2.8g potassium chloride, to be placed in grinding in ball grinder 50min after being sufficiently mixed, obtain Mixture B;Being mixed by mixture A and B, be placed in square porcelain boat, total mixture amount is less than 2/3rds of porcelain boat total amount.
Two, pretreatment
The mixture of gained in step one is placed in vacuum drying oven, after 150 DEG C of heat treatment 20h;
Three, solid state reaction
Gained mixture in step 2 is placed in the middle of tube furnace boiler tube, is passed through nitrogen protection, is warming up to 1000 DEG C, heating rate It is 20 DEG C/min, after reaching target temperature, is incubated 40min, naturally cools to room temperature, take out.
Four, product washing
Porcelain boat product in step 3 is taken out, is placed in 500ml beaker, add deionized water, excusing from death stirring 30min, use The filter membrane of 0.5M carries out vacuum filtration, again adds deionized water, repeated washing step, altogether washing 3-5 time.Products therefrom is placed in Air dry oven is dried 24h.
Embodiment 3:
One, raw material is prefabricated
Weigh 0.4g glucose, the ammonium chloride of 0.5g, 0.05g nickel nitrate, after being sufficiently mixed in glove box, it is placed in agate mortar Middle grinding 60min, obtains mixture A;Weigh 13.5g sodium chloride and 11.5g potassium chloride, to be placed in ball mill after being sufficiently mixed Grind 60min, obtain mixture B;Being mixed by mixture A and B, be placed in square porcelain boat, total mixture amount is total less than porcelain boat 2/3rds of amount.
Two, pretreatment
The mixture of gained in step one is placed in vacuum drying oven, after 200 DEG C of heat treatment 30h, after being naturally down to room temperature Take out;
Three, solid state reaction
Gained mixture in step 2 is placed in the middle of tube furnace boiler tube, is passed through nitrogen protection, is warming up to 1300 DEG C, heating rate It is 30 DEG C/min, after reaching target temperature, is incubated 60min, naturally cools to room temperature, take out.
Four, product washing
Porcelain boat product in step 3 is taken out, is placed in 500ml beaker, add deionized water, excusing from death stirring 30min, use The filter membrane of 0.5M carries out vacuum filtration, again adds deionized water, repeated washing step, altogether washing 3-5 time.Products therefrom is placed in Air dry oven is dried 24h.
The technique concrete material characterization of gained sample using the present invention refers to shown in Figure of description 1 and accompanying drawing 2.
Above detailed description of the invention is only the preferred embodiment of this creation, not in order to limit this creation, all in this wound Any modification, equivalent substitution and improvement etc. done within the spirit made and principle, should be included in this creation protection domain it In.

Claims (9)

1. the method preparing graphene/nanometer nickel composite material, it is characterised in that: it uses one-step synthesis, including such as Lower processing step:
1), glucose and nickel nitrate are mixed, grinds in agate mortar;
2), sodium chloride and potassium chloride are mixed, through ball mill ball milling;
3), by step 1) and 2) in the material mixing that obtains uniform, and the pre-heat treatment;
4), the mixing material after the pre-heat treatment is placed in square porcelain boat, porcelain boat is positioned over the centre position of tube furnace, is passed through Inert gas shielding, calcines under certain heating rate;
5), isothermal holding is carried out after calcining;
6), under inert gas shielding, it is naturally cooling to room temperature, takes out sample;
7), gained mixture deionized water is cleaned, and obtains product by vacuum filtration.
The method preparing graphene/nanometer nickel composite material the most as claimed in claim 1, it is characterised in that: in step 1), institute The mass ratio stating glucose and nickel nitrate is (1-16): 1.
The method preparing graphene/nanometer nickel composite material the most as claimed in claim 1, it is characterised in that: step 2) in, institute The mass ratio stating sodium chloride and potassium chloride is (1-3): 1.
The method preparing graphene/nanometer nickel composite material the most as claimed in claim 1, it is characterised in that: in step 3), in advance The temperature of heat treatment is 80 DEG C-200 DEG C.
The method preparing graphene/nanometer nickel composite material the most as claimed in claim 1, it is characterised in that: in step 4), rise Temperature speed is 5 DEG C-30 DEG C/min;Calcining heat is 950 DEG C-1300 DEG C;Described noble gas is nitrogen.
The method preparing graphene/nanometer nickel composite material the most as claimed in claim 1, it is characterised in that: in step 5), institute Stating temperature retention time is 30min-60min.
The method preparing graphene/nanometer nickel composite material the most as claimed in claim 1, it is characterised in that: in step 6), will Mixture is placed in beaker, adds deionized water, excusing from death stirring 30min, uses the filter membrane of 0.5M to carry out vacuum filtration, repeat to wash Wash step 3-5 time;Products therefrom is placed in air dry oven and is dried 24h.
The method preparing graphene/nanometer nickel composite material the most as claimed in claim 1, it is characterised in that: in step 1), Portugal Needing to add ammonium chloride in the mixture of grape sugar and nickel nitrate, the mass ratio of described glucose and ammonium chloride is 4:5.
The method preparing graphene/nanometer nickel composite material the most as claimed in claim 1, it is characterised in that: in step 1), Portugal Grape sugar 0.1g, nickel nitrate 0.1g, grind 50min;Step 2) in, sodium chloride 11.4g and potassium chloride 2.8g, grinds 50min;Step 3) in, 150 DEG C of the pre-heat treatment 20h;In step 4), being warming up to 1000 DEG C, heating rate is 20 DEG C/min, is incubated 40min.
CN201610266045.2A 2016-04-25 2016-04-25 A method of preparing graphene/nanometer nickel composite material Expired - Fee Related CN105935777B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109304475A (en) * 2017-07-28 2019-02-05 中国石油化工股份有限公司 Carbon-coating nickel composite material and preparation method
CN113677177A (en) * 2021-08-12 2021-11-19 广西大学 Preparation method and wave-absorbing application of graphene-based metal composite material

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109304475A (en) * 2017-07-28 2019-02-05 中国石油化工股份有限公司 Carbon-coating nickel composite material and preparation method
CN113677177A (en) * 2021-08-12 2021-11-19 广西大学 Preparation method and wave-absorbing application of graphene-based metal composite material
CN113677177B (en) * 2021-08-12 2023-11-21 广西大学 Preparation method of graphene-based metal composite material and wave absorbing application thereof

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