CN102604593B - Cubic-phase nickel nanostructure-graphene complex and preparation method thereof - Google Patents
Cubic-phase nickel nanostructure-graphene complex and preparation method thereof Download PDFInfo
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- CN102604593B CN102604593B CN201210071724.6A CN201210071724A CN102604593B CN 102604593 B CN102604593 B CN 102604593B CN 201210071724 A CN201210071724 A CN 201210071724A CN 102604593 B CN102604593 B CN 102604593B
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Abstract
The invention provides a magnetic nanomaterial-graphene complex, in particular to a cubic-phase nickel nanostructure-graphene complex, the chemical formula of which is c-Ni/GN. A preparation method for the cubic-phase nickel nanostructure-graphene complex includes the following steps that: (a) graphite oxide is dissolved in 2-pyrrolidone or N-methylpyrrolidone, so that brown solution is obtained; (b) acetylacetone nickel and octadecylamine are added into the brown solution, the brown solution is heated to 110 DEG C to 140 DEG C under the protection of nitrogen, and the temperature is kept for 20 to 40 minutes, then increased to 202 DEG C and kept for 1.5 to 2.5 hours; (c) organic solvent is added to suddenly stop reaction, and the temperature of the reaction system is rapidly decreased to the room temperature; (d) reaction product is separated out, washed and dried. The cubic-phase nickel nanostructure-graphene complex provided by the invention is a novel electromagnetic wave-absorbing material, and enhances the wave-absorbing property of nickel, so that nickel has good electromagnetic wave-absorbing property. The preparation method for the cubic-phase nickel nanostructure-graphene complex is simple, convenient and quick, the effect of reduction is good, the raw materials are easy to obtain, and the cost is low.
Description
Technical field
The present invention relates to electromagnetic wave absorbent material field, be specifically related to a kind of Emission in Cubic nickel nanostructure-Graphene complex body and preparation method thereof.
Background technology
In recent years, wireless communication technique is fast-developing in business, industry and military industry, when offering convenience for our life, also brought electromagnetic harm, this make preparation can the device of electromagnetic wave absorption and the task of the material of research electromagnetic wave absorption become more urgent.Therefore the research that, hertzian wave is had to wide absorption region, high absorptive capacity, low density, thermostability is good, resistance of oxidation is a good material arouses great concern.
Metallic nickel is a kind of typical magneticsubstance, and it has good potential application at aspects such as hydrogen storage materials, catalyzer, Magnetic Sensor and electromagnetic wave absorbent materials.
Graphene (GN) is owing to having good electroconductibility, large many good character such as specific surface area, snappiness and chemical stability, so be usually used as the substrate of other active materials of carrying.Since the people such as Geim in 2004 find Graphene, the research of Graphene and other nano material complex bodys arouses great concern, and wherein these nano materials mainly comprise various nanoparticles, for example, and Mn
3o
4, MoS
2, Fe
3o
4, Co, Co
3o
4, Co (OH)
2, CoFe
2o
4, Ni (OH)
2nanoparticle and NiO nanoparticle.Because Graphene has very high electric conductivity, metal nickel nano particle has good magnetic simultaneously, if metal nickel nano grain and Graphene can be made to complex body, so this matrix material will have good absorption of electromagnetic wave effect.In addition, compare with traditional absorbing material, Graphene has that density is little, erosion resistance good, flexibility is large and low cost and other advantages, so this makes to have more realistic meaning for the research of metallic nickel-Graphene electromagnetic wave absorption material.
Summary of the invention
The problem that the present invention solves is to provide a kind of Emission in Cubic nickel nanostructure-Graphene complex body, has good absorption of electromagnetic wave performance.The application also provides the preparation method of this Emission in Cubic nickel nanostructure-Graphene complex body, easy, and fast, reduction effect is good.
In order to solve the problems of the technologies described above, technical scheme of the present invention is:
Magnetic Nano material-Graphene complex body, is characterized in that, chemical formula is c-Ni/GN.
The preparation method of the magnetic Nano material-Graphene complex body described in more than one, comprising:
A) graphite oxide is dissolved in to 2-Pyrrolidone or N-Methyl pyrrolidone, obtains brown solution;
B) acetylacetonate nickel and stearylamine are added in above-mentioned brown solution, under nitrogen protection, be heated to 110 ℃～140 ℃ and maintain 20min～40min, then be warming up to 202 ℃ and maintain 1.5h～2.5h;
C) add organic solvent to stop reaction is sudden, make the temperature of reaction system be down to rapidly room temperature;
D) reaction product isolated, dry after washing, obtain c-Ni/GN.
As preferably, the concentration that described graphite oxide is dissolved in graphite oxide in the solution that 2-Pyrrolidone or N-Methyl pyrrolidone obtain is 0.8g/L～1.5g/L.
As preferably, the mass ratio of described graphite oxide and acetylacetonate nickel is 1: 35～45.
As preferably, the mass ratio of described graphite oxide and stearylamine is 1: 90～120.
As preferably, described c) organic solvent in is alcohols.
As preferably, described d) in, washing is for being used the alternately washing of normal hexane, acetone.
As preferably, described d) in, be dried as dry under 40 ℃ of vacuum.
Emission in Cubic nickel nanostructure-Graphene complex body provided by the invention is a kind of novel electromagnetic wave absorbent material, and the absorbing property of nickel is improved, and has good absorption of electromagnetic wave performance.The preparation method of this Emission in Cubic nickel nanostructure-Graphene complex body has easy, and fast, reduction effect is good, and starting material are easy to get, low cost and other advantages.
Accompanying drawing explanation
Fig. 1 is the graphite (a) of using in the embodiment of the present invention, GO (b), the GN (c) of preparation and the XRD figure of c-Ni (2-P)/GN (d), c-Ni (NMP)/GN (e);
Fig. 2 is TEM (a), HRTEM (b) and SAED (c) photo of the Graphene prepared of the embodiment of the present invention;
Fig. 3 is TEM (a-c), HRTEM (d) and FFT (illustration in the d) figure of c-Ni (2-P)/GN of preparing of the embodiment of the present invention;
Fig. 4 is the TEM figure (a, b) of the c-Ni (NMP) for preparing of the embodiment of the present invention, and TEM figure (c, d), HRTEM figure (e, f), the high resolution lattice phase (upper end illustration in f) of c-Ni (NMP)/GN, FFT scheme (lower end illustration in f);
Fig. 5 is the c-Ni (2-P), the c-Ni (2-P) that prepare of the embodiment of the present invention/GN, c-Ni (NMP), the microwave reflection rate loss value figure of c-Ni (NMP)/GN when 3mm thickness.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, rather than limiting to the claimed invention.
The invention provides a kind of magnetic Nano material-Graphene complex body, is Emission in Cubic nickel nanostructure-Graphene complex body, and chemical formula is c-Ni/GN.
The preparation method of c-Ni/GN provided by the invention comprises the following steps:
A) graphite oxide (GO) is dissolved in to 2-Pyrrolidone (2-P) or N-Methyl pyrrolidone (NMP), obtains brown solution, the concentration of graphite oxide is 0.8g/L～1.5g/L, and graphite oxide is prepared by improved Hummers method;
B) acetylacetonate nickel and stearylamine are added in above-mentioned brown solution, under nitrogen protection, be heated to 110 ℃～140 ℃ and maintain 20min～40min, then be warming up to 202 ℃ and maintain 1.5h～2.5h; In solution, the mass ratio of graphite oxide and acetylacetonate nickel is 1: 35～45, and the mass ratio of graphite oxide and stearylamine is 1: 90～120;
C) add organic solvent to stop reaction is sudden, make the temperature of reaction system be down to rapidly room temperature, organic solvent can be used alcohols, as ethanol;
D) after reaction product isolated, wash, can be separated by centrifugal mode, preferably use normal hexane, acetone to replace washed product, then dry, preferably dry under 40 ℃ of vacuum, obtain c-Ni/GN.
Wherein, the c-Ni/GN preparing when using 2-Pyrrolidone (2-P) for solvent is spherical Face-centred Cubic Metals nickel-graphite alkene complex body, is designated as c-Ni (2-P)/GN herein; The c-Ni/GN preparing when using N-Methyl pyrrolidone (NMP) for solvent is flower-shaped Face-centred Cubic Metals nickel-graphite alkene complex body, is designated as c-Ni (NMP)/GN herein.
Similar with the above-mentioned method of preparing complex body, if do not introduce Graphene, can prepare spherical face-centered cubic phase metallic nickel simple substance and flower-shaped face-centered cubic phase metallic nickel.
Embodiment:
1, prepare graphite oxide
Adopt improved Hummers method to prepare graphite oxide, as the raw material of preparing Emission in Cubic metallic nickel-Graphene complex body.
Take 5g Graphite Powder 99,5gNaNO
3, and the dense H of 230mL
2sO
4, be placed in ice-water bath, slowly add while stirring 30gKMnO
4, about 15 minutes of this process.
Remove ice-water bath, put into 35 ℃ of water-baths, slowly add 460mL distilled water, this process approximately 30 minutes, product graduates into brown by black.
Be put in afterwards in 98 ℃ of oil baths and be incubated 15 minutes.
Withdraw from after oil bath, add 1400mL warm water, stir, add 100mLH
2o
2, now product becomes golden yellow.Filter, the rare HCl solution washing that is 5% with massfraction, in filtrate without SO
4 2-till.Products therefrom is in 70 ℃ of air dryings.
2, prepare spherical Face-centred Cubic Metals nickel-graphite alkene complex body
20mgGO is added in 20mL2-pyrrolidone, and ultrasonic dispersion, obtains brown solution.
Next; 2mmol acetylacetonate nickel and 2g stearylamine are added in above-mentioned brown solution; first mixture is heated to 120 ℃ and maintain 30min in this temperature; then increase the temperature to 202 ℃; in this temperature, maintain 2h; whole reaction process is carried out under the protection of nitrogen, and keeps magnetic agitation always.
After reaction stops, adding 20mL ethanol to stop reaction is sudden, make the temperature of reaction system be reduced to rapidly room temperature.
Finally, by centrifugal mode, isolate reaction product, and alternately wash with normal hexane, acetone, product, in 40 ℃ of vacuum-dryings, makes c-Ni (2-P)/GN.
3, prepare flower-shaped Face-centred Cubic Metals nickel-graphite alkene complex body
C-Ni (2-P)/GN is similar to preparation, just by 2-Pyrrolidone, changes solvent into N-Methyl pyrrolidone, makes c-Ni (NMP)/GN.
In addition, use the same method but do not introduce Graphene, preparing Emission in Cubic metallic nickel simple substance c-Ni (2-P) and c-Ni (NMP).
Sign to product:
1, the GO of the graphite of using in embodiment, preparation, GN, c-Ni (2-P)/GN and c-Ni (NMP)/GN are characterized, please refer to Fig. 1, Fig. 1 is the graphite (a) of using in the embodiment of the present invention, GO (b), the GN (c) of preparation and the XRD figure of c-Ni (2-P)/GN (d), c-Ni (NMP)/GN (e).
From figure (a), selected graphite raw material crystallinity is good, locates to occur the diffraction peak of (002) crystal face in 2 θ=26.5 °, and corresponding interlamellar spacing is 0.34nm.After oxidation, products therefrom GO still has good crystallinity, and maintenance laminate structure, but diffraction peak moves to low angle, in 2 θ=10.9 °, locate to occur diffraction peak, respective layer spacing is 0.76nm, sees figure (b), the oxidized rear introducing oxygen-containing functional group of graphite, thus the increase of interlamellar spacing caused.Figure (c) is the XRD figure of the rear products therefrom GN of graphite oxide reduction, from figure, do not observe the diffraction peak that interlamellar spacing is 0.76nm, and in 2 θ=23.5 °, there is diffraction peak a little less than in the of and broadening to occur, show that GO is reduced, and the laminate structure of Graphene is destroyed.Figure (d) XRD diffracting spectrum (e) all coincide with JCPDS card 65-2865, shows that gained metal Ni is face-centred cubic structure (a=b=c=3.524nm).In addition, similar with figure (c), owing to having added graphite oxide, figure (d) all observes the diffraction peak weak and broadening of locating 2 θ=23.5 ° in (e) and occurs, but do not occur that interlamellar spacing is the diffraction peak of 0.76nm, in the process that shows to generate at metal Ni, GO is reduced to Graphene.
2, please refer to Fig. 2, Fig. 2 be the Graphene prepared of the embodiment of the present invention TEM (transmission electron microscope, a), HRTEM (high resolution transmission electron microscopy, b) and SAED (selected area electron diffraction, c) photo.Figure a schemes for obtained the TEM of Graphene by graphite oxide reduction, therefrom can find out, after peroxidation and reduction, the laminate structure of graphite is destroyed, but gained Graphene still keeps sheet structure, observe some folds simultaneously, may be because the too thin reason of Graphene.Figure b and c are respectively HRTEM photo and the SAED collection of illustrative plates of Graphene, from figure b, can find out, gained Graphene is individual layer, and laminate thickness is 0.34nm, and this is that 0.34nm is corresponding with the interlamellar spacing of graphite (002) face.From figure c, can find out, in Graphene, carbon atom is taked sp2 hydridization, is plane polynuclear plane, has complete crystalline structure.
3, please refer to Fig. 3, Fig. 3 is TEM (a-c), HRTEM (d) and FFT (fast Fourier transform, illustration in the d) figure of c-Ni (2-P)/GN of preparing of the embodiment of the present invention.By figure a and b, can be found out, the Emission in Cubic nickel (c-Ni) of preparation is spherical, and diameter dimension is between 50 to 200nm, and what these nanometer balls were random is distributed on graphene sheet layer.In addition, from figure c, can observe the edge that Graphene is corroded by nickel nano particle, show that c-Ni nanometer ball deep " inlaying " is in Graphene, and these diameters nanometer ball offspring that the nano particle 10 to 20nm forms by some diameters that is 200nm.The edge that can observe Graphene in figure d, wherein the spacing of lattice of metallic nickel is 0.203nm, coincide with the d value of (111) face diffraction peak in Emission in Cubic metallic nickel XRD figure spectrum.Two-dimensional FFT (fast fourier transform) figure that in figure d, illustration is Graphene, shows as six side's diffraction lattices of typical Graphene, thereby further proves that products therefrom is the complex body of metallic nickel and Graphene.
4, please refer to Fig. 4, Fig. 4 is the TEM figure (a, b) of the c-Ni (NMP) for preparing of the embodiment of the present invention, and TEM figure (c, d), HRTEM figure (e, f), the high resolution lattice phase (upper end illustration in f) of c-Ni (NMP)/GN, FFT scheme (lower end illustration in f).By the method similar to preparing c-Ni (NMP)/GN, just do not introduce Graphene, can make flower-shaped face-centered cubic phase metallic nickel c-Ni (NMP), figure a, b are the TEM figure of c-Ni (NMP), as can be seen from the figure, products therefrom is flower-shaped.In addition, from high magnification TEM photo b, can find out, these flower-shaped nickel nano particles are actually by diameter the offspring that the little nano particle between 10-20nm forms.In figure c, d, can find out, flower-shaped nickel nano particle is attached on Graphene uniformly, and can see clearly the edge of the two, as shown in the direction of arrow in figure.Figure can observe the edge that Graphene is corroded by metallic nickel in e, shows nickel nano particle being embedded in Graphene tightly.Figure can see the hexagonal lattice phase of carbon sp2 hydridization in lattice edge that c-Ni (NMP) is regular and Graphene in f.In addition, the spacing of lattice that can measure nickel from high resolution TEM figure is 0.203nm, and (111) face of corresponding Emission in Cubic nickel is consistent with XRD result before.
5,, in order to assess the absorption of electromagnetic wave performance of c-Ni (2-P)/GN, c-Ni (NMP)/GN complex body, related compound magnetic permeability and specific inductivity test have been carried out.Test is carried out under fixing frequency and thickness of sample, and reflectivity loss value (RL) calculates according to conveyer line theory, and formula is as follows:
RL(dB)＝20log(Z
in-Z
0)/(Z
in+Z
0)| (2)
Wherein f represents microwave frequency, and d represents the thickness of absorption agent, and c represents the light velocity, Z
inrepresent the input resistance of absorption agent.
In 1.0-18.0GHz range of frequency, measure related compound magnetic permeability and specific inductivity, as shown in Figure 5, Fig. 5 is the c-Ni (2-P), the c-Ni (2-P) that prepare of the embodiment of the present invention/GN, c-Ni (NMP), the microwave reflection rate loss value figure of c-Ni (NMP)/GN when 3mm thickness to result.As seen from the figure, the Emission in Cubic complex body of prepared two kinds of nickel and Graphene all shows than the better absorption of electromagnetic wave efficiency of corresponding nickel monomer.For example, c-Ni (2-P) nanometer ball is observed two place's absorption peaks in 1.0-18.0GHz range of frequency, respectively at 9.0GHz and 12.8GHz place, corresponding be respectively-2.4dB of RL and-3.1dB, c-Ni (2-P)/GN complex body has obvious absorption at 9.0GHz place, corresponding RL is-9.0dB that comparing nickel simple substance has the absorption of enhancing; For c-Ni (NMP) flower-like nanometer particle and complex body thereof, the absorption peak that also observes two place's wide regions in 1.0-18.0GHz range of frequency absorbs, respectively at 8.0GHz and 9.2GHz place, and corresponding be respectively-7.9dB of RL and-9.0dB.From the above results, can find out, c-Ni/GN complex body has better electromagnetic performance, thereby shows stronger absorption of electromagnetic wave ability, thereby makes it be expected to the absorbing material as microwave shielding device.
Above Emission in Cubic nickel nanostructure-Graphene complex body provided by the present invention and preparation method thereof is described in detail.Applied specific case herein principle of the present invention and embodiment are set forth, the explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Claims (7)
1. a preparation method for nano material-Graphene complex body, is characterized in that, comprising:
A) graphite oxide is dissolved in to 2-Pyrrolidone or N-Methyl pyrrolidone, obtains brown solution;
B) acetylacetonate nickel and stearylamine are added in above-mentioned brown solution, under nitrogen protection, be heated to 110 ℃～140 ℃ and maintain 20min～40min, then be warming up to 202 ℃ and maintain 1.5h～2.5h;
C) add organic solvent to stop reaction is sudden, make the temperature of reaction system be down to rapidly room temperature;
D) reaction product isolated, dry after washing, obtain c-Ni/GN.
2. preparation method according to claim 1, is characterized in that, the concentration that described graphite oxide is dissolved in graphite oxide in the solution that 2-Pyrrolidone or N-Methyl pyrrolidone obtain is 0.8g/L～1.5g/L.
3. preparation method according to claim 1, is characterized in that, the mass ratio of described graphite oxide and acetylacetonate nickel is 1:35～45.
4. preparation method according to claim 1, is characterized in that, the mass ratio of described graphite oxide and stearylamine is 1:90～120.
5. preparation method according to claim 1, is characterized in that, described c) in organic solvent be alcohols.
6. preparation method according to claim 1, is characterized in that, described d) middle washing as using normal hexane, acetone alternately to wash.
7. preparation method according to claim 1, is characterized in that, described d) in be dried as dry under 40 ℃ of vacuum.
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| RU2570672C1 (en) * | 2014-05-13 | 2015-12-10 | Федеральное государственное бюджетное образовательное учреждение высшего профессионального образования "Кемеровский государственный университет" (КемГУ) | Method of producing of composite material of carbon-nickel system |
| CN104084575B (en) * | 2014-06-30 | 2016-03-23 | 北京师范大学 | Emission in Cubic cobalt/graphene composite material, preparation method and absorbing property |
| CN104084576B (en) * | 2014-06-30 | 2016-03-23 | 北京师范大学 | Six side's phase cobalt/graphene composite materials, preparation method and absorbing property |
| CN104043840B (en) * | 2014-07-01 | 2016-03-23 | 北京师范大学 | Emission in Cubic cobalt-nickel alloy nano-cluster-graphene composite material, Preparation Method And The Use |
| CN104117683B (en) * | 2014-07-01 | 2016-03-23 | 北京师范大学 | Six side's phase cobalt-nickel alloy nano-cluster-graphene composite materials, Preparation Method And The Use |
| CN104357788B (en) * | 2014-10-30 | 2017-01-25 | 安徽鼎恒再制造产业技术研究院有限公司 | Ni-Gr-B nano-coating and preparation method thereof |
| CN105880618A (en) * | 2015-01-12 | 2016-08-24 | 冯云 | Preparation method for composite mesoporous material with nano nickel loaded on graphene |
| CN106554006B (en) * | 2015-09-25 | 2019-07-02 | 国家纳米科学中心 | A kind of carbon material, preparation method and applications |
| CN105817648B (en) * | 2016-04-29 | 2017-10-17 | 北京师范大学 | Iron-nickel alloy nano-cluster graphene composite material, preparation method and the usage |
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