CN106683813B - A kind of graphene coated can be changed phase nano magnetic composite materials and preparation method thereof - Google Patents
A kind of graphene coated can be changed phase nano magnetic composite materials and preparation method thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/0036—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
- H01F1/0045—Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
- H01F1/0054—Coated nanoparticles, e.g. nanoparticles coated with organic surfactant
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/10—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure
- H01F1/11—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles
- H01F1/112—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials non-metallic substances, e.g. ferrites, e.g. [(Ba,Sr)O(Fe2O3)6] ferrites with hexagonal structure in the form of particles with a skin
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
- H01F1/34—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites
- H01F1/36—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials non-metallic substances, e.g. ferrites in the form of particles
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
Abstract
The present invention provides a kind of variable phase nano magnetic composite materials of graphene coated, and it is graphene shell to have nucleocapsid, shell, is made of multi-layer graphene piece, shell thickness 5-50nm；Core is magnetic core, is the nano magnetic particle that particle diameter can be changed for 10-90nm phases.The present invention also proposes that the graphene coated can be changed the preparation method of phase nano magnetic composite materials.Method proposed by the present invention, using plasma as synthetic environment, reduces the toxicity and environmental pollution that reactant is brought, is conducive to mass production using ferrocene powder as source of iron and carbon source.Nitrogenous ratio by regulating and controlling preparation process plasma can control the object phase of obtained magnetic nanoparticle.It is tiny by the nano-magnetic powder diameter of the graphene coated prepared by the approach, be evenly distributed, good sphericity, and preparation flow is brief.
Description
Technical field
The invention belongs to nano-function powder material and Preparation Technique of Powders fields, and in particular to a kind of composite graphite alkene
Functional material and preparation method thereof.
Background technology
Graphene (Graphene) is a kind of plane forming hexangle type in honeycomb lattice by carbon atom with sp2 hybridized orbits
Film, only there are one the two-dimentional carbon materials of carbon atom thickness.Graphene has strong toughness, electrical conductance and thermal conductivity.Iron and iron
Nitrogen compound has excellent magnetic property, but its chemical stability is poor, especially iron phase.Using graphene as covering material
The chemical stability of magnetic-particle and the problem of electrical conductance difference can be improved very well so that this composite material can answer well
Used in magnetic fluid, targeted drug, electromagnetic wave absorbent material, electromagnetic shielding material, oxidation reduction catalyst, fine ceramics material and
The multiple fields such as lithium battery.
In presently disclosed patent and document, report it is mostly be carbon-coated metallic nano-particles preparation method, such as be pyrolyzed
Method, arc process, infusion process, CVD method etc. obtain carbon-encapsulated iron nano particle；For the iron nitride nanometer of graphene coated
Grain can be directly obtained there is no a kind of method.
Application publication number is CN101347455A, and date of publication is on January 21st, 2009, and a kind of entitled carbon-encapsulated iron of patent is received
Rice corpuscles and its as treatment liver-cancer medicine carrier application, a kind of carbon-encapsulated iron nanoparticles have been invented, especially by straight
Galvanic electricity arc method prepares.
Application publication number is CN102623696A, and date of publication is August in 2012 1, patent name：A kind of core-shell type cladding
Nitrided iron nano-complex particle preparation method and application, have invented a kind of core-shell type carbon coating nitrided iron nano-complex particle system
Standby technique, especially using the carbon-encapsulated iron nano particle of direct-current plasma fabricated in situ as presoma, using nitridation work
Skill obtains carbon coating nitrided iron nano-complex particle.
Application publication number is CN101710512A, and date of publication is on May 19th, 2010, the entitled graphene of patent and carbon coating
Ferromagnetic nano metal composite material and preparation method.It has invented one kind by graphene and carbon-coated ferromagnetic nano
Grain, and provide a kind of special CVD method and prepare this kind of composite powder material.
These methods all have the advantages that deficiency that is respective, but also having more, as testing equipment is complicated, preparation condition is tight
Lattice, flow are cumbersome etc., cause manufacturing cost higher, to influence the exploitation that graphene/carbon coats iron and iron nitride powder
With application.
Invention content
In view of the above-mentioned present state of the art, the object of the present invention is to provide a kind of graphene coateds can be changed phase nanometer
Magnetic composite.
The present invention also aims to provide a kind of preparation side of the variable phase nano magnetic composite materials of graphene coated
Method, and this method can regulate and control the object facies type of magnetic core by regulating and controlling the nitrogenous ratio of preparation process plasma.
Realize that the technical solution of above-mentioned purpose of the present invention is：
A kind of variable phase nano magnetic composite materials of graphene coated, it is graphene shell to have nucleocapsid, shell, by
Multi-layer graphene piece forms, shell thickness 5-50nm；Core is magnetic core, is that particle diameter is variable for 10-90nm phases
Nano magnetic particle.
Wherein, the phase of the nano magnetic particle is α-Fe, the γ-Fe and γ-Fe (N), γ '-Fe of iron phase4N、ε-
Fe3N、α”-Fe16N2It is one or more in the iron nitride of phase.
The present invention also proposes that the graphene coated can be changed the preparation method of phase nano magnetic composite materials, including with
Lower step：
(1) after continuous and multiple plasma generation device reaction cavity carries out inert gas purge, with indifferent gas
Body is full of entire reaction cavity, completely cuts off air；
(2) it is excited after obtaining stable inert gas plasma stream by plasma electrical source, by inputting reaction gas
Source forms hybrid plasma stream, then by ferrocene powder thermal evaporation, and ferrocene steam is sent into plasma in the form of current-carrying gas
Body central area；
(3) the high enthalpy of plasma and chemical activation effect are utilized, after ferrocene to be pyrolyzed rapidly to concurrent biochemical reaction,
It grows up by forming core to obtain nano magnetic particle and in particle surface coated graphite alkene in plasma flame stream tail portion；
(4) reaction chamber is dropped into room temperature under the conditions of inert gas shielding, the composite granule collected, as graphene
Coat nano magnetic particle composite material.
Plasma method prepares the variable phase nano magnetic particle of graphene coated and prepares particle compared with other methods
Degree is smaller, particle diameter distribution is uniform and can obtain the magnetic core of not jljl phase by controlling the nitrogenous ratio in plasma.This hair
It is bright to use ferrocene (C10H10Fe it is) reaction raw materials, promotes to react by plasma, directly obtaining graphene coated can be covert
State nano magnetic particle composite granule.
Wherein, using ferrocene (C10H10Fe) as source of iron and carbon source, the evaporation fluidized bed temperature setting of ferrocene powder is
100~400 DEG C；The current-carrying gas be argon gas, nitrogen, ammonia it is one or more.
Further, the plasma stream is inductive coupled plasma stream, capacitively coupled plasma stream and micro-
One kind in wave coupled plasma stream, is mixed to form by inert gas and reactant gas source, reactant gas source and inert gas
Molar ratio is 0~5:1；The inert gas is argon gas, helium, one or more in neon, reactant gas source be hydrogen,
It is one or more in nitrogen, ammonia.
Wherein, the nitrogenous ratio that plasma is controlled by adjusting the flow of reactant gas source, inert gas and current-carrying gas, from
And control the phase composition of nano magnetic particle so that the phase of nano magnetic particle is α-Fe, γ-Fe, γ-Fe (N), γ '-
Fe4N、ε-Fe3N、α”-Fe16N2In it is one or more.
One of the preferred technical solution of the present invention is：The plasma it is nitrogenous than (it is always former that nitrogen-atoms accounts for plasma
The molar ratio of son amount) when being 0, the phase of the nano magnetic particle in gained composite material is in α-Fe and the γ-Fe of iron phase
It is one or two kinds of.
The present invention another optimal technical scheme be：When the nitrogenous ratio of the plasma is 5~80%, gained composite wood
The phase of nano magnetic particle in material is γ-Fe (N), γ '-Fe4N、ε-Fe3It is one or more in N.
The advantage of the invention is that：
(1) method proposed by the present invention, using ferrocene powder as source of iron and carbon source, using plasma as synthesis ring
Border reduces toxicity and environmental pollution that reactant is brought, is conducive to mass production.
(2) object of obtained magnetic nanoparticle can be controlled by regulating and controlling the nitrogenous ratio of preparation process plasma
Phase.
(3) tiny by the carbon-coated nano-magnetic powder diameter prepared by the approach, be evenly distributed, good sphericity,
And preparation flow is brief.
Graphene coated prepared by the method for the present invention mutually can have goodization by abnormal nano magnetic composite materials simultaneously
Stability, magnetic property and electrical property are learned, therefore in targeted drug, magnetic fluid, absorbing material, lithium battery material and catalyst etc. are more
A field has a wide range of applications potentiality.
Description of the drawings
Fig. 1 be the graphene coated that is prepared of embodiment 1, embodiment 2 and embodiment 3 can mutually metamorphosis nano-magnetic it is compound
The XRD spectrum of material.
Fig. 2 is the particle diameter distribution and TEM figures that graphene coated prepared by embodiment 1 can be changed phase nano particle composite material
Fig. 3 is the TEM figures that graphene coated prepared by embodiment 2 can be changed phase nano particle composite material.
Fig. 4 is the TEM figures that graphene coated prepared by embodiment 3 can be changed phase nano particle composite material.
Specific implementation mode
The content that following embodiment further illustrates the present invention, but should not be construed as limiting the invention.
Ink alkene cladding proposed by the present invention can be changed the preparation method of phase nano magnetic composite materials, include the following steps：
(1) after continuous and multiple plasma generation device reaction cavity carries out inert gas purge, with indifferent gas
Body is full of entire reaction cavity, completely cuts off air；
(2) it is excited after obtaining stable inert gas plasma stream by plasma electrical source, by inputting reaction gas
Source forms hybrid plasma stream, then by ferrocene powder thermal evaporation, and ferrocene steam is sent into plasma in the form of current-carrying gas
Body central area；
(3) the high enthalpy of plasma and chemical activation effect are utilized, after ferrocene to be pyrolyzed rapidly to concurrent biochemical reaction,
It grows up by forming core to obtain nano magnetic particle and in particle surface coated graphite alkene in plasma flame stream tail portion；
(4) reaction chamber is dropped into room temperature under the conditions of inert gas shielding, the composite granule collected, as graphene
Coat nano magnetic particle composite material.
The equipment used can be existing plasma generating equipment, in embodiment, specifically use patent
Equipment disclosed in CN104851548A.
Unless otherwise instructed, the means used in embodiment are this field conventional technology.
The concrete technology of the preparation of the variable phase nano magnetic composite materials of graphene coated is as follows in embodiment：
Embodiment 1：
Using commercially available ferrocene powder as raw material, repeatedly with after argon purge reaction cavity, gas is formed as plasma using argon gas and is built
The argon plasma of vertical stable operation, wherein argon flow amount are 5slpm, and it is 5slpm that gas argon flow amount is protected on side.Constant temperature fluidized bed temperature
Degree is set as 120 DEG C, ferrocene steam is sent into plasma flame stream by the argon gas that flow is 3slpm, by plasma
Body pyrolytic and priming reaction obtain graphene coated and can be changed phase nano magnetic particle, the XRD diagram of product as shown in Figure 1,
TEM schemes and particle diameter distribution is as shown in Figure 2.
As shown in Figure 1, the object phase composition of embodiment 1 is α-Fe, γ-Fe and C.As shown in Figure 2, the graphene coated obtained
Variable phase nano magnetic composite materials particle diameter distribution is between 10~90nm, and average grain diameter is in 26.3nm.Particle is in ball substantially
It shape or spheroid shape and is coated by shell, it is respectively 20nm and 5nm to measure core diameter and shell thickness about.By the crystalline substance to nucleocapsid
Interlamellar spacing measures discovery, and the interplanar distance of shell is about 0.35nm, close with the interplanar distance in (002) face of graphene,
This illustrates that shell is collectively constituted by multi-layer graphene piece；The interplanar distance of core is 0.203nm, (110) interplanar distance with α-Fe
And/or (111) interplanar distance of γ-Fe is close, this is consistent with XRD data.Composite material even particle size distribution, sphericity
It is good.
Embodiment 2：
Using commercially available ferrocene powder as raw material, after repeatedly using argon purge reaction cavity, using argon gas and nitrogen as plasma shape
Establish the argon-nitrogen plasma of stable operation jointly at gas, wherein argon flow amount is 5slpm, nitrogen flow 1slpm, side protection
Gas argon flow amount is 10slpm.Constant temperature fluidized bed is set as 160 DEG C, and carrier gas flux is the argon gas of 1slpm, other operate same embodiment
1.The XRD diagram of graphene coated nitrided iron nano magnetic particle is obtained as shown in Figure 1, TEM figures are as shown in Figure 3.
As shown in Figure 1, the object phase composition for the product that prepared by embodiment 2 is γ-Fe (N), γ '-Fe4N、ε-Fe3N.By Fig. 3
As it can be seen that obtained graphene coated can be changed phase nano magnetic composite materials particle diameter distribution between 10~90nm, have apparent
Nucleocapsid, the graphene sheet layer of core outer cladding multilayer.Being evenly distributed of composite material, good sphericity.
Embodiment 3：
Using commercially available ferrocene powder as raw material, after repeatedly using argon purge reaction cavity, using argon gas and nitrogen as plasma shape
Establish the argon nitrogen radio frequency plasma of stable operation jointly at gas, wherein argon flow amount is 5slpm, nitrogen flow 3slpm, side
Protection gas argon flow amount is 10slpm.Constant temperature fluidized bed is set as 180 DEG C, other operations are the same as embodiment 2.Obtain graphene coated nitrogen
Change the XRD diagram of iron nano magnetic particle as shown in Figure 1, TEM figures are as shown in Figure 4.
As shown in Figure 1, the object phase composition of embodiment 3 is γ-Fe (N), ε-Fe3N.From fig. 4, it can be seen that obtained graphene packet
Variable phase nano magnetic composite materials particle diameter distribution is covered between 10~110nm, and there is apparent nucleocapsid, core outsourcing
Cover the graphene sheet layer of multilayer.Being evenly distributed of composite material, good sphericity.
Although above having used general explanation, specific implementation mode and experiment, the present invention is made to retouch in detail
It states, but on the basis of the present invention, some can be made to it and modified or improved, this is aobvious and easy to those skilled in the art
See.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (7)
1. a kind of graphene coated can be changed the preparation method of phase nano magnetic composite materials, which is characterized in that the graphite
It is graphene shell that alkene cladding, which can be changed phase nano magnetic composite materials to have nucleocapsid, shell, is made of multi-layer graphene piece,
Shell thickness is 5 ~ 50nm；Core is magnetic core, is the nano magnetic particle that particle diameter can be changed for 10 ~ 90nm phases；
The preparation method, includes the following steps：
(1) it after continuous and multiple plasma generation device reaction cavity carries out inert gas purge, is filled with inert gas
Full entire reaction cavity, completely cuts off air；
(2) it is excited after obtaining stable inert gas plasma stream by plasma electrical source, by inputting reactant gas source shape
At hybrid plasma stream, then by ferrocene powder thermal evaporation, ferrocene steam is sent into plasma in the form of current-carrying gas
Heart district domain；
(3) the high enthalpy of plasma and chemical activation effect are utilized, after ferrocene to be pyrolyzed rapidly to concurrent biochemical reaction, is being waited
It grows up to obtain nano magnetic particle and in particle surface coated graphite alkene by forming core in gas ions flame stream tail portion；
(4) reaction chamber is dropped into room temperature under the conditions of inert gas shielding, the composite granule collected, as graphene coated
Nano magnetic particle composite material.
2. preparation method according to claim 1, which is characterized in that the phase of the nano magnetic particle is the α-of iron phase
Fe, γ-Fe and γ-Fe (N), γ '-Fe4N、ε-Fe3N、α’’-Fe16N2It is one or more in the iron nitride of phase.
3. preparation method according to claim 1, which is characterized in that use ferrocene（C10H10Fe）As source of iron and carbon
The evaporation fluidized bed temperature setting in source, ferrocene powder is 100 ~ 400 DEG C；The current-carrying gas be argon gas, nitrogen, ammonia one kind or
It is a variety of.
4. preparation method according to claim 1, which is characterized in that the plasma stream is inductive coupled plasma
One kind in body stream, capacitively coupled plasma stream, microwave coupling plasma jet mixing shape by inert gas and reactant gas source
At the molar ratio of reactant gas source and inert gas is 0 ~ 5:1；The inert gas is one in argon gas, helium, neon
Kind is a variety of, and reactant gas source is one or more in hydrogen, nitrogen, ammonia.
5. preparation method according to claim 1, which is characterized in that by adjusting reactant gas source, inert gas and current-carrying
The flow of gas controls the nitrogenous ratio of plasma, to control the phase composition of nano magnetic particle so that nano-magnetic
The phase of grain is α-Fe, γ-Fe, γ-Fe (N), γ '-Fe4N、ε-Fe3N、α’’-Fe16N2In it is one or more.
6. preparation method according to claim 5, which is characterized in that when the nitrogenous ratio of the plasma is 0, gained
The phase of nano magnetic particle in composite material is one or both of α-Fe, the γ-Fe of iron phase.
7. preparation method according to claim 5, which is characterized in that when the nitrogenous ratio of the plasma is 5 ~ 80%,
The phase of nano magnetic particle in gained composite material is γ-Fe (N), γ '-Fe4N、ε-Fe3It is one or more in N.
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| CN107127335B (en) * | 2017-05-18 | 2019-04-02 | 山东大学 | A kind of preparation method of hud typed carbon-encapsulated iron nanocomposite |
| CN109215913B (en) * | 2017-07-04 | 2021-03-02 | 中国科学院金属研究所 | Method for preparing carbon-coated iron nitride and composite magnetic nano material thereof |
| CN107895653B (en) * | 2017-10-27 | 2019-10-25 | 西安理工大学 | Microwave prepares cigarette filter/graphene composite material method and application thereof |
| CN108110231B (en) * | 2017-12-05 | 2020-05-19 | 银隆新能源股份有限公司 | Carbon-coated Fe4N nano composite material, preparation method and application thereof |
| CN108659790A (en) * | 2018-04-26 | 2018-10-16 | 南通大学 | A kind of preparation method of the composite wave-suction material of magnetic-particle intercalation porous graphene |
| CN110575814A (en) * | 2019-08-27 | 2019-12-17 | 中国科学院合肥物质科学研究院 | Graphene-coated metal-based environment functional material and preparation method and application thereof |
| CN111724954B (en) * | 2020-02-07 | 2023-01-20 | 宴晶科技(北京)有限公司 | Graphene oxide magnetic bead, antibody-coupled graphene oxide magnetic bead and application of graphene oxide magnetic bead in cell sorting |
| CN113231633B (en) * | 2021-04-06 | 2022-09-20 | 北京碳垣新材料科技有限公司 | Graphene copper-based composite powder and preparation method thereof |
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