CN101710512B - Composite material of graphene and carbon-encapsulated ferromagnetic nano metal and preparation method thereof - Google Patents
Composite material of graphene and carbon-encapsulated ferromagnetic nano metal and preparation method thereof Download PDFInfo
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- CN101710512B CN101710512B CN2009100732333A CN200910073233A CN101710512B CN 101710512 B CN101710512 B CN 101710512B CN 2009100732333 A CN2009100732333 A CN 2009100732333A CN 200910073233 A CN200910073233 A CN 200910073233A CN 101710512 B CN101710512 B CN 101710512B
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Abstract
The invention provides a composite material of graphene and carbon-encapsulated ferromagnetic nano metal and a preparation method thereof. The composite material is composed of grapheme material and carbon-encapsulated ferromagnetic nano metallic particles evenly loaded on the surface of the grapheme material, the grapheme material is composed of monolayer graphite with thickness smaller than 50nm, the carbon-encapsulated ferromagnetic nano metallic particle has a diameter of 2-100nm, ferromagnetic metal can be one of ferrum, cobalt and nickel or more than two of ferrum, cobalt and nickel in any proportion, the weight ratio of metal to carbon is 1-20:1. The invention takes graphite as the carrier to evenly load the magnetic metallic primer on the surface of the graphite so as to prepare the carbon-encapsulated ferromagnetic nano metallic particles evenly scattered in the surface of the grapheme, so that the carbon-encapsulated ferromagnetic nano metallic particles has good magnetic performance and electrical conductivity, and can have wide application prospect in such fields as magnetic separation catalyst, sewage disposal, electromagnetic shielding and wave absorbing, etc.
Description
Technical field
What the present invention relates to is a kind of composite material, the present invention also relates to a kind of preparation methods that meets.Be specifically related to a kind of Graphene/carbon-encapsulated ferromagnetic nano metal composite material and preparation method thereof
Background technology
The carbon-encapsulated ferromagnetic metal nanoparticle is meant that with magnetic metal nanoparticles such as iron, cobalt, nickel be core, and the outside coats the concentric layered shell polysaccharide graphite-structure and a kind of composite material with Nano capsule structure of forming.Owing to coated carbon-coating in metal nanoparticle outside, therefore medium-term and long-term stable at air, Heat stability is good has solved nano metal oxidation and problem of unstable easily in air.At the magnetic seal fluid, fields such as magnetic ink and magnetic separating catalyst, electromagnetic shielding and suction ripple have widely uses.
The preparation method of carbon-encapsulated ferromagnetic nano metal generally has arc discharge method, chemical vapour deposition technique, pyrolysismethod, liquid impregnation carbonizatin method and explosion method etc.At present, chemical vapour deposition technique is widely used in the preparation of carbon-clad metal nano material so that its equipment is simple, easy to operate, cost is low.This method is in reative cell, and nano metal to be coated or its compound particle are dispersed on the substrate, feeds carbon source at a certain temperature, and the latter pyrolytic reaction takes place and be deposited as carbon to form clad structure under the catalytic action of metallic particles.For example in the thunder emerging grade with the so-gel Supercritical Drying Technology synthetic contain the bimetallic SiO of Fe, Co
2Nanoporous aerogel is a catalyst, adopts CVD method high temperature gas phase catalytic cracking methane to synthesize C-(the Fe-Co)/SiO of carbon-encapsulated iron cobalt
2Nano composite material [Lei Zhongxing, Liu Jing, the carbon coating of .CVD methods such as Li Xuanke preparation (Fe, Co) structure of nano particle and electromagnetic property. magnetic material and device:, 2003,34 (4): 4-6.].
Graphene (graphene) is the newfound in recent years a kind of carbonaceous new material by the tightly packed one-tenth bi-dimensional cellular of monolayer carbon atom shape lattice structure, Graphene has excellent electricity, calorifics and mechanical property and high specific area, is expected in the acquisition extensive use of fields such as high-performance electronic device, composite material, field emmision material, environmental protection, catalyst carrier and electronic shield.
Summary of the invention
The object of the present invention is to provide a kind of have good magnetic property and good electrical conductivity, Graphene and the carbon-encapsulated ferromagnetic nano metal composite material that can use in fields such as magnetic separating catalyst, sewage disposal, electromagnetic shielding and suction ripples.The present invention also aims to provide the preparation method of a kind of Graphene and carbon-encapsulated ferromagnetic nano metal composite material.
The object of the present invention is achieved like this:
Graphene of the present invention and carbon-encapsulated ferromagnetic nano metal composite material are made up of at the carbon-encapsulated ferromagnetic nano metal particle on grapheme material surface grapheme material and uniform load, described grapheme material form by mono-layer graphite and thickness less than 50nm, described carbon-encapsulated ferromagnetic nano metal particle diameter is 2～100nm, described ferromagnetic metal is that any one or the two or more arbitrary proportion in iron, cobalt, the nickel mixes, and the weight ratio of metal and carbon is 1～20: 1.
The preparation method of Graphene of the present invention and carbon-encapsulated ferromagnetic nano metal composite material is:
With concentration is that the ultrasonic dispersion 0.5～5h of graphite oxide solution of 0.1～10mg/mL prepares the graphene oxide dispersion liquid, be with concentration to be the ferromagnetic metal salting liquid of 0.1～5mol/L add in graphene oxide dispersion liquid at 0.1～100: 1 by the soluble-salt of ferromagnetic metal and graphite oxide weight ratio then, stir 0.5～10h, be to be made into solution that concentration be 0.1～5mol/L at 1～20: 1 with precipitation reagent by the mol ratio of itself and transition metal soluble-salt then, and its speed with 1～10mL/min joined in the above-mentioned graphite oxide dispersion liquid that is dissolved with the ferromagnetic metal soluble salt, react 0.5～10h at 0～100 ℃ under the vigorous stirring, through suction filtration, fully washing, promptly make composite granule after the drying, speed with 5～50 ℃/min under its nitrogen or the argon atmospher is warming up to 500～800 ℃, feed hydrogen and the carbon-source gas gaseous mixture that flow velocity is 10～100mL/min then and carry out chemical vapour deposition (CVD) 1～60min, under nitrogen or argon atmospher, room temperature is reduced in reaction then, take out composite granule, promptly get Graphene/carbon-encapsulated ferromagnetic nano metal composite material.
Described ferromagnetic metal is any one or the two or more combination in any in iron, cobalt, the nickel.
Described ferromagnetic metal soluble-salt is wherein any one of nitrate, acetate, chloride, sulfate.
Described precipitation reagent is any one in ammoniacal liquor, NaOH, potassium hydroxide, sodium carbonate, sodium acid carbonate, the ammoniacal liquor.
Described carbon-source gas is any one in carbon monoxide, methane, acetylene, the ethene.
The ratio of described hydrogen and carbon-source gas is 0.1～10: 1.
The present invention is carrier with the grapheme material, with magnetic Nano metal precursor uniform load on its surface, prepared the carbon-encapsulated ferromagnetic nano metal particle that is dispersed in the Graphene surface by chemical vapour deposition technique then, make it have good magnetic property and good electrical conductivity simultaneously, be expected to be with a wide range of applications in fields such as magnetic separating catalyst, sewage disposal, electromagnetic shielding and suction ripples.
Compared with prior art, the present invention has following advantage:
Prepared graphene of the present invention/carbon-encapsulated ferromagnetic nano metal composite material has good conductivity and magnetic property simultaneously, therefore is with a wide range of applications in fields such as magnetic separating catalyst, sewage disposal, electromagnetic shielding and suction ripples.
Description of drawings
Fig. 1 is Graphene/carbon-encapsulated ferromagnetic nano metal composite material electronic transmission electromicroscopic photograph of embodiment 3.
Fig. 2 is Graphene/carbon-encapsulated ferromagnetic nano metal composite material XRD spectra of embodiment 3.
Fig. 3 is the table with test results 1 of each embodiment.
Embodiment
For example the present invention is done in more detail below and describes:
With 100mL concentration is that the ultrasonic dispersion of the graphite oxide solution 5h of 0.1mg/mL prepares the graphene oxide dispersion liquid, presses Fe (NO then
3)
2With the graphite oxide weight ratio be that 0.1: 1 ratio is the Fe (NO of 0.1mol/L with concentration
3)
2Solution adds in the graphene oxide dispersion liquid, stirs 0.5h, then with precipitation reagent sodium carbonate by itself and Fe (NO
3)
2Mol ratio be to be made into solution that concentration be 0.1mol/L at 1: 1, and its speed with 1mL/min is joined the above-mentioned Fe of being dissolved with (NO
3)
2The graphite oxide dispersion liquid in, under the vigorous stirring at 0 ℃ of reaction 0.5h, through suction filtration, fully promptly make the catalyst composite granule after washing, the drying.Then prepared powder speed with 5 ℃/min under blanket of nitrogen is warming up to 600 ℃, feed hydrogen and the carbon mono oxide mixture that flow velocity is 10mL/min then and carry out chemical vapour deposition (CVD) 1min, promptly get required Graphene/carbon-encapsulated ferromagnetic nano metal composite material.Wherein the volume ratio of hydrogen and carbon monoxide is 0.1: 1, and specific performance is seen Fig. 3.
With 100mL concentration is that the ultrasonic dispersion of the graphite oxide solution 5h of 10mg/mL prepares the graphene oxide dispersion liquid, presses CoCl then
2With the graphite oxide weight ratio be that 100: 1 ratio is the CoCl of 5mol/L with concentration
2Salting liquid adds in the graphene oxide dispersion liquid, stirs 10h, then with precipitation reagent urea by itself and CoCl
2Mol ratio be to be made into solution that concentration be 5mol/L at 20: 1, and its speed with 10mL/min is joined the above-mentioned CoCl of being dissolved with
2The graphite oxide dispersion liquid in, under the vigorous stirring at 100 ℃ of reaction 10h, through suction filtration, fully promptly make the catalyst composite granule after washing, the drying.Then prepared powder speed with 10 ℃/min under argon atmospher is warming up to 500 ℃, feed hydrogen and the methane blended gas that flow velocity is 100mL/min then and carry out chemical vapour deposition (CVD) 60min, promptly get required Graphene/carbon-encapsulated ferromagnetic nano metal composite material.Wherein the volume ratio of hydrogen and methane is 10: 1, and specific performance is seen Fig. 3.
With 100mL concentration is that the ultrasonic dispersion of the graphite oxide solution 2h of 1mg/mL prepares the graphene oxide dispersion liquid, presses Ni (CH then
3COO)
2With the graphite oxide weight ratio be that 20: 1 ratio is the Ni (CH of 1mol/L with concentration
3COO)
2Salting liquid adds in the graphene oxide dispersion liquid, stirs 2h, then with precipitation reagent ammoniacal liquor by itself and Ni (CH
3COO)
2Mol ratio be to be made into solution that concentration be 2mol/L at 10: 1, and its speed with 5mL/min is joined the above-mentioned Ni of being dissolved with (CH
3COO)
2The graphite oxide dispersion liquid in, under the vigorous stirring at 20 ℃ of reaction 3h, through suction filtration, fully promptly make the catalyst composite granule after washing, the drying.Then prepared powder speed with 30 ℃/min under argon atmospher is warming up to 800 ℃, the feeding flow velocity is that hydrogen and the ethene gaseous mixture of 50mL/min carries out chemical vapour deposition (CVD) 1min, promptly gets required Graphene/carbon-encapsulated ferromagnetic nano metal composite material.Wherein the volume ratio of hydrogen and ethene is 0.1: 1, and specific performance is seen Fig. 3.
With 100mL concentration is that the ultrasonic dispersion of the graphite oxide solution 3h of 2mg/mL prepares the graphene oxide dispersion liquid, presses Ni (NO then
3)
2And Co (NO
3)
2With the graphite oxide weight ratio be that 40: 1 ratio is the Ni (NO of 2mol/L with concentration
3)
2And Co (NO
3)
2Mixing salt solution add in the graphene oxide dispersion liquid, stir 2h, wherein Ni (NO
3)
2With Co (NO
3)
2Mol ratio be 1: 1.Then with precipitation reagent NaOH by itself and Ni (NO
3)
2And Co (NO
3)
2The mol ratio of salt-mixture be to be made into solution that concentration be 1mol/L at 2: 1, and its speed with 5mL/min is joined the above-mentioned Ni of being dissolved with (NO
3)
2And Co (NO
3)
2The graphite oxide dispersion liquid of salt-mixture in, under the vigorous stirring at 30 ℃ of reaction 4h, through suction filtration, fully promptly make the catalyst composite granule after washing, the drying.Then prepared powder speed with 20 ℃/min under argon atmospher is warming up to 600 ℃, the feeding flow velocity is that hydrogen and the acetylene gaseous mixture of 50mL/min carries out chemical vapour deposition (CVD) 20min, promptly gets required Graphene/carbon-encapsulated ferromagnetic nano metal composite material.Wherein the volume ratio of hydrogen and acetylene is 1: 1, and specific performance is seen Fig. 3.
With 100mL concentration is that the ultrasonic dispersion of the graphite oxide solution 0.5h of 5mg/mL prepares the graphene oxide dispersion liquid, presses Ni (NO then
3)
2And Fe (NO
3)
2With the graphite oxide weight ratio be that 10: 1 ratio is the Ni (NO of 1mol/L with concentration
3)
2And Fe (NO
3)
2Mixing salt solution add in the graphene oxide dispersion liquid, stir 4h, wherein Ni (NO
3)
2With Fe (NO
3)
2Mol ratio be 2: 1.Then with precipitation reagent potassium hydroxide by itself and Ni (NO
3)
2And Fe (NO
3)
2The mol ratio of salt-mixture be to be made into solution that concentration be 2mol/L at 2: 1, and its speed with 5mL/min is joined the above-mentioned Ni of being dissolved with (NO
3)
2And Fe (NO
3)
2The graphite oxide dispersion liquid of salt-mixture in, under the vigorous stirring at 30 ℃ of reaction 5h, through suction filtration, fully promptly make the catalyst composite granule after washing, the drying.Then prepared powder speed with 50 ℃/min under argon atmospher is warming up to 700 ℃, the feeding flow velocity is that hydrogen and the ethene gaseous mixture of 70mL/min carries out chemical vapour deposition (CVD) 30min, promptly gets required Graphene/carbon-encapsulated ferromagnetic nano metal composite material.Wherein the volume ratio of hydrogen and ethene is 0.1: 1, and specific performance is seen Fig. 3.
Claims (7)
1. Graphene and carbon-encapsulated ferromagnetic nano metal composite material, it is characterized in that: form at the carbon-encapsulated ferromagnetic nano metal particle on grapheme material surface by grapheme material and uniform load, described grapheme material form by mono-layer graphite and thickness less than 50nm, described carbon-encapsulated ferromagnetic nano metal particle diameter is 2～100nm, described ferromagnetic metal is that any one or the two or more arbitrary proportion in iron, cobalt, the nickel mixes, and the weight ratio of metal and carbon is 1～20: 1.
2. the preparation method of Graphene and carbon-encapsulated ferromagnetic nano metal composite material is characterized in that:
With concentration is that the ultrasonic dispersion 0.5～5h of graphite oxide solution of 0.1～10mg/mL prepares the graphene oxide dispersion liquid, be with concentration to be the ferromagnetic metal salting liquid of 0.1～5mol/L add in graphene oxide dispersion liquid at 0.1～100: 1 by the soluble-salt of ferromagnetic metal and graphite oxide weight ratio then, stir 0.5～10h, be to be made into solution that concentration be 0.1～5mol/L at 1～20: 1 with precipitation reagent by the mol ratio of the soluble-salt of itself and ferromagnetic metal then, and its speed with 1～10mL/min joined in the above-mentioned graphite oxide dispersion liquid that is dissolved with the ferromagnetic metal soluble salt, react 0.5～10h at 0～100 ℃ under the vigorous stirring, through suction filtration, fully washing, promptly make composite granule after the drying, with it under nitrogen or argon atmospher, speed with 5～50 ℃/min is warming up to 500～800 ℃, feed hydrogen and the carbon-source gas gaseous mixture that flow velocity is 10～100mL/min then and carry out chemical vapour deposition (CVD) 1～60min, under nitrogen or argon atmospher, room temperature is reduced in reaction then, take out composite granule, promptly get the composite material of Graphene and carbon-encapsulated ferromagnetic nano metal.
3. the preparation method of Graphene according to claim 2 and carbon-encapsulated ferromagnetic nano metal composite material is characterized in that: described ferromagnetic metal is any one or the two or more combination in any in iron, cobalt, the nickel.
4. the preparation method of Graphene according to claim 3 and carbon-encapsulated ferromagnetic nano metal composite material is characterized in that: described ferromagnetic metal soluble-salt is wherein any one of nitrate, acetate, chloride, sulfate.
5. the preparation method of Graphene according to claim 4 and carbon-encapsulated ferromagnetic nano metal composite material is characterized in that: described precipitation reagent is any one in ammoniacal liquor, NaOH, potassium hydroxide, sodium carbonate, the sodium acid carbonate.
6. the preparation method of Graphene according to claim 5 and carbon-encapsulated ferromagnetic nano metal composite material is characterized in that: described carbon-source gas is any one in carbon monoxide, methane, acetylene, the ethene.
7. the preparation method of Graphene according to claim 6 and carbon-encapsulated ferromagnetic nano metal composite material is characterized in that: the ratio of described hydrogen and carbon-source gas is 0.1～10: 1.
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Granted publication date: 20110914 Termination date: 20171120 |