CN105513740A - Spinel type ferromagnet/graphene nanometer composite material, preparing method and application thereof - Google Patents

Spinel type ferromagnet/graphene nanometer composite material, preparing method and application thereof Download PDF

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Publication number
CN105513740A
CN105513740A CN201510884428.1A CN201510884428A CN105513740A CN 105513740 A CN105513740 A CN 105513740A CN 201510884428 A CN201510884428 A CN 201510884428A CN 105513740 A CN105513740 A CN 105513740A
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salt
graphene
composite material
preparation
crystal formation
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赵雪伶
***
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Shanghai Polytechnic University
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Shanghai Polytechnic University
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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

Abstract

The invention belongs to the technical field of nanometer function materials and particularly provides a spinel type ferromagnet/graphene nanometer composite material, a preparing method and application thereof. According to the method, an improved Hummers method is adopted for preparing graphene oxide, and then a one-step in-situ method is adopted for synthesizing the spinel type ferromagnet/graphene nanometer composite material. The method has the advantages that the raw materials needed by the preparing method are low in cost, the preparation technology is simple, the composite material can be prepared on a large scale, and the method is suitable for large-scale production and application. The obtained composite material has good simulating peroxidase activity and can be used for detecting micromolecule hydrogen peroxide (H2O2), glucose and the like.

Description

A kind of sharp crystal formation is ferromagnetic/graphene nanocomposite material, preparation method and application thereof
Technical field
The present invention relates to nano-functional material synthesis technical field, specifically, relate to a kind of sharp crystal formation ferromagnetic/graphene nanocomposite material, preparation method and application thereof.
Background technology
From Fe in 2007 3o 4since nano particle is in the news and has class peroxidase activity, ferriferous oxide magnetic Nano material occupies very important status in class peroxidase activity nano materials research field.Based on the class peroxidase activity that it is outstanding, ferriferous oxide magnetic Nano material is widely used in the research fields such as pollutant process, environmental monitoring, bio-sensing.Although Fe 3o 4nano particle possess with low cost, preparation technology simple, can accomplish scale production, biocompatibility and the advantage such as Evaluation of Biocompatibility is good, but Fe 3o 4nano particle is owing to wherein containing ferrous ion (Fe 2+), be very easily oxidized in storing process after the production, cause the change of the character such as original magnetic property and catalytic activity, be unfavorable for research and apply steady in a long-term.
The MFe of cubic spinel structure 2o 4(M=Co, Mn, Zn, Ni, Cu etc.) are a kind of important ferriferous oxide magnetic Nano materials, and wherein oxygen atom defines face-centered cubic closs packing, M 2+the Fe of ion and half 3+ion is in occupation of octahedral interstice site, in addition half Fe 3+ion is in occupation of tetrahedral site.Bivalent metal ion instead of Fe 3o 4middle Fe 2+define MFe 2o 4compound, these compounds effectively can stop Fe 2+aerial oxidation.MFe 2o 4because of the performance of its uniqueness, as less particle diameter, larger specific area, superparamagnetism and high saturation magnetization etc. become the focus that nanosecond science and technology field is paid close attention to, in biological medicine, and drug delivery, environment remediation, catalysis, the new visual field has been opened up in the fields such as magnetic response radiography.
But not modified sharp crystal formation ferromagnetic particle is easy to reunite, and extremely unstable, its application is also faced with huge challenge.In the recent period, the researcher such as Lanzhou University Su finds to keep its chemism by the reunion that is bundled in by nano particle between the method prevention nano particle in particular substrate.When the nano particle of zero dimension being loaded in the nano material of one dimension or two dimension, the nanostructure of this hydridization not only can keep the performance of their original homogenous material, and can show better synergy.
Graphene be exactly a kind of by carbon atom with sp 2hybridized orbit composition hexangle type be the flat film of honeycomb lattice, is the two-dimensional material only having a carbon atom thickness, because the electricity of its uniqueness, heat, machinery and chemical property are all the focus studied in recent years in various fields.Graphene and ferriferous oxide magnetic nanoparticle are carried out compound, from the angle of the structure of matter, composite material can have following advantage: (1) ferriferous oxide magnetic nanoparticle adheres to or is distributed on graphene film, not only can suppress the reunion of magnetic nanoparticle and the curling of Graphene, but also the effective area of Graphene can be increased; (2) graphene film is as the one-tenth paralinin of ferriferous oxide magnetic nanoparticle, can the nucleation of induced nano crystalline substance and growth distribution, forms meticulous nanostructure, is disperseed equably and control form at graphenic surface by chemical functional; (3) no matter be that magnetic nanoparticle is attached on Graphene, or Graphene support particles can form perfect overall structure, and this structure is a kind of conductive network, can shorten the approach of electronics and ion transportation.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of sharp crystal formation ferromagnetic/graphene nanocomposite material, preparation method and application thereof.The cost of raw material needed for this preparation method is cheap, and preparation technology is simple, can prepare in enormous quantities, be suitable for large-scale production and application.It can solve the problem of existing sharp crystal formation ferriferous oxide magnetic nanoparticle poor stability, and meanwhile, it also can improve Mimetic enzyme activity greatly, for detecting Small molecular hydrogen peroxide, glucose.
In the present invention with graphene oxide, trivalent iron salt and ferrous iron magnetic metal salt for raw material, by adding NaOH/DEG storing solution as reducing agent, hydro-thermal reaction one step prepares sharp crystal formation ferromagnetic/graphene nanocomposite material.Concrete technical scheme is as follows.
The invention provides a kind of sharp crystal formation ferromagnetic/graphene nanocomposite material, this nano composite material is composited by ferriferous oxide magnetic nanoparticle and Graphene, ferriferous oxide magnetic nanoparticle uniform particle diameter, narrowly distributing.
The present invention also provide a kind of sharp crystal formation ferromagnetic/preparation method of graphene nanocomposite material, concrete steps are as follows:
(1) first 0.03-0.3g graphene oxide is joined the reaction unit filling 20-200mL diglycol solvent
In, ultrasonic 1-5h, makes graphene oxide be dispersed in solvent;
(2) then, in reaction unit, add 0.12-1.2g solubility trivalent iron salt and ferrous iron magnetic metal salt stirs, under inert gas shielding, at 190-220 DEG C of temperature, add thermal agitation 0.5-2h; Wherein: described ferrous iron magnetic metal salt is Zn salt, Co salt, Ni salt, Mn salt or Cu salt;
(3) last, the 10-100mg/mLNaOH/DEG storing solution of 5-50mL is joined rapidly in said mixture,
At 190-220 DEG C of temperature, react 1-5h, product centrifugation and washing after, obtain sharp crystal formation ferromagnetic/graphene nanocomposite material.
In above-mentioned steps (1), graphene oxide take graphite as raw material, adopts the Hummers method improved to prepare.
In above-mentioned steps (2), the mol ratio of solubility trivalent iron salt and ferrous iron magnetic metal salt is 2:1.
In above-mentioned steps (2), solubility trivalent iron salt is selected from Fe (NO 3) 3, FeCl 3or Fe 2(SO 4) 3in one or more.
In above-mentioned steps (2), in ferrous iron magnetic metal salt, Zn salt is selected from ZnCl 2, ZnSO 4, Zn (NO 3) 2or Zn (CH 3cOO) 2in any one; Co salt is selected from CoCl 2, CoSO 4, Co (NO 3) 2or Co (CH 3cOO) 2in any one; Ni salt is selected from NiCl 2, NiSO 4, Ni (NO 3) 2or Ni (CH 3cOO) 2in any one; Mn salt is selected from MnCl 2, MnSO 4, Mn (NO 3) 2or Mn (CH 3cOO) 2in any one; Cu salt is selected from CuCl 2, CuSO 4, Cu (NO 3) 2or Cu (CH 3cOO) 2in any one.
In above-mentioned steps (3), 0.2-2g NaOH NaOH is joined in 20-200mL diglycol DEG, under inert atmosphere protection, at 120-150 DEG C of temperature, stir 1-2h, be then cooled to 70 DEG C and make NaOH/DEG storing solution.
The present invention further provides above-mentioned sharp crystal formation ferromagnetic/application of graphene nanocomposite material in Small molecular hydrogen peroxide, glucose detection.
Compared with prior art, the invention has the advantages that:
1. replace Fe with ferrous iron magnetic metal salt in the present invention 2+participate in reaction, effectively can stop Fe 2+aerial oxidation, prepare stable sharp crystal formation ferromagnetic/graphene nanocomposite material;
2. the cost of raw material needed for preparation method provided by the invention is cheap, and preparation technology is simple, can prepare in enormous quantities;
3. in preparation method provided by the invention diglycol not only as solvent but also as reducing agent, without the need to other reducing agents;
4. the sharp crystal formation for preparing of the present invention ferromagnetic/graphene nanocomposite material good dispersion, ferriferous oxide magnetic nanoparticle is evenly distributed at graphenic surface, structured size;
5. the sharp crystal formation for preparing of the present invention ferromagnetic/graphene nanocomposite material has good Mimetic enzyme active, can be used for the monitoring of Small molecular hydrogen peroxide, glucose etc.
Accompanying drawing explanation
Fig. 1 is the crystal structure schematic diagram of sharp crystal formation ferriferous oxide magnetic nanoparticle.
Fig. 2 is the sharp crystal formation Fe that embodiment 1 obtains 3o 4transmission electron microscope (TEM) photo of/rGO nano composite material.
Fig. 3 is the sharp crystal formation Fe that embodiment 1 obtains 3o 4x-ray diffraction (XRD) figure of/rGO nano composite material.
Fig. 4 is the sharp crystal form M nFe that embodiment 3 obtains 2o 4x-ray diffraction (XRD) figure of/rGO nano composite material.
Fig. 5 is the cyclic voltammetric linear scan diagram of embodiment 8.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in more detail.
Fig. 1 is the crystal structure schematic diagram of sharp crystal formation ferriferous oxide magnetic nanoparticle.
The sharp crystal formation Fe of embodiment 1 3o 4the preparation of/rGO nano composite material
(1) preparation of graphene oxide
Use the Hummers method improved to prepare graphene oxide, concrete grammar is as follows: first, takes 0.75g graphite powder and joins in 250mL round-bottomed flask, then adds 100mL sulfuric acid/phosphoric acid mixing material (volume ratio: 9:1) wherein; After magnetic agitation is even, slowly add 4.5g potassium permanganate; Subsequently, mixture adds thermal agitation 12h in 50 DEG C; After pre-oxidation product is cooled to room temperature, slowly add 300mL deionized water, dropwise add in 3mL30% hydrogen peroxide under agitation and unreacted potassium permanganate; Place its sedimentation of half angel, after the supernatant liquor that inclines, supercentrifuge centrifugation; Finally use deionized water and 5% hydrogen peroxide washing precipitation to neutral;
(2) join in 20mL diglycol (DEG) by 0.2g NaOH (NaOH), under nitrogen protection, 120-150 DEG C adds thermal agitation 1-2h, is then cooled to 70 DEG C and makes NaOH/DEG storing solution;
(3) 0.03g graphene oxide is joined in the reaction unit filling 20mL diglycol solvent, ultrasonic 1h, make graphene oxide be dispersed in solvent;
(4) in reaction unit, 0.12gFeCl is added again 3, under mixture nitrogen protection, 190-220 DEG C adds thermal agitation 1h;
(5) joined rapidly in said mixture by 5mLNaOH/DEG storing solution, add thermal response 1h at 190-220 DEG C, product centrifugation also, after washing, obtains Fe 3o 4/ rGO nano composite material.
Fig. 2 is sharp crystal formation Fe prepared by embodiment 1 3o 4the transmission electron microscope photo of/rGO nano composite material, as can be seen from the figure, Fe 3o 4magnetic nanoparticle is dispersed in graphenic surface uniformly, and uniform particle diameter.
Fig. 3 is sharp crystal formation Fe prepared by embodiment 1 3o 4the X-ray diffractogram of/rGO nano composite material.
The sharp crystal formation Fe of embodiment 2 3o 4/ rGO nano composite material
By the soluble ferric iron salt FeCl in the step (4) of embodiment 1 3with Fe (NO 3) 3or Fe 2(SO 4) 3replace, other steps and condition are all identical with embodiment 1, can prepare sharp crystal formation Fe equally 3o 4/ rGO nano composite material.
The sharp crystal form M nFe of embodiment 3 2o 4the preparation of/rGO nano composite material
In the step (4) of embodiment 1, except soluble ferric iron salt FeCl 3, then add the ferrous iron magnetic metal salt (mol ratio of ferric iron and ferrous iron magnetic metal salt is fixing 2:1) containing Mn outward, comprise MnCl 2, MnSO 4, Mn (NO 3) 2or Mn (CH 3cOO) 2in one, other steps and condition are all identical with embodiment 1, and actual conditions does corresponding variation and adjustment in the scope that summary of the invention limits, and can obtain sharp crystal form M nFe 2o 4/ rGO nano composite material.Fig. 4 is the sharp crystal form M nFe that embodiment 3 obtains 2o 4x-ray diffraction (XRD) figure of/rGO nano composite material.
The sharp crystal formation ZnFe of embodiment 4 2o 4the preparation of/rGO nano composite material
In the step (4) of embodiment 1, except soluble ferric iron salt FeCl 3, then add the ferrous iron magnetic metal salt (mol ratio of ferric iron and ferrous iron magnetic metal salt is fixing 2:1) containing Zn outward, comprise ZnCl 2, ZnSO 4, Zn (NO 3) 2or Zn (CH 3cOO) 2in one, other steps and condition are all identical with embodiment 1, and actual conditions does corresponding variation and adjustment in the scope that summary of the invention limits, and can obtain sharp crystal formation ZnFe 2o 4/ rGO nano composite material.
The sharp crystal C oFe of embodiment 5 2o 4the preparation of/rGO nano composite material
In the step (4) of embodiment 1, except soluble ferric iron salt FeCl 3, then add the ferrous iron magnetic metal salt containing Co outward, comprise C DEG C of l 2, CoSO 4, Co (NO 3) 2or Co (CH 3cOO) 2in one, other steps and condition are all identical with embodiment 1, and actual conditions does corresponding variation and adjustment in the scope that summary of the invention limits, and can obtain sharp crystal C oFe 2o 4/ rGO nano composite material.
The sharp crystal formation NiFe of embodiment 6 2o 4the preparation of/rGO nano composite material
In the step (4) of embodiment 1, except soluble ferric iron salt FeCl 3, then add the ferrous iron magnetic metal salt (mol ratio of ferric iron and ferrous iron magnetic metal salt is fixing 2:1) containing Ni outward, comprise NiCl 2, NiSO 4, Ni (NO 3) 2or Ni (CH 3cOO) 2in one, other steps and condition are all identical with embodiment 1, and actual conditions does corresponding variation and adjustment in the scope that summary of the invention limits, and can obtain sharp crystal formation NiFe 2o 4/ rGO nano composite material.
The sharp crystal C uFe of embodiment 7 2o 4the preparation of/rGO nano composite material
In the step (4) of embodiment 1, except soluble ferric iron salt FeCl 3, then add the ferrous iron magnetic metal salt (mol ratio of ferric iron and ferrous iron magnetic metal salt is fixing 2:1) containing Cu outward, comprise CuCl 2, CuSO 4, Cu (NO 3) 2or Cu (CH 3cOO) 2in one, other steps and condition are all identical with embodiment 1, and actual conditions does corresponding variation and adjustment in the scope that summary of the invention limits, and can obtain sharp crystal C uFe 2o 4/ rGO nano composite material.
The sharp crystal formation Fe of embodiment 8 3o 4the peroxidase activity of/rGO nano composite material detects
(1) by glass-carbon electrode washed with de-ionized water 3-5 time, smooth surface is made, the grain of described aluminium oxide with aluminum oxide polishing powder polishing
Footpath is followed successively by 1 μm, 0.3 μm, 50nm, the sharp crystal formation Fe prepared by Example 1 3o 4/ rGO nano composite material, adds absolute ethyl alcohol ultrasonic disperse and makes suspension, then gets suspension 10 μ L and is added drop-wise on the glass-carbon electrode of having polished, after vacuumize, obtain sharp crystal formation Fe 3o 4the electrode that/rGO nano composite material is modified;
(2) with sharp crystal formation Fe 3o 4the electrode that/rGO nano composite material is modified is work electrode, and saturated calomel electrode is reference electrode,
Gauze platinum electrode is to electrode, and composition three-electrode system, carries out electro-chemical test.In 15mLPBS cushioning liquid (pH=7.4), in the voltage range of-0.9V-1V, under adding and do not add the condition of hydrogen peroxide, carry out cyclic voltammetric linear scan with the speed of 0.05V/s.
Experimental result as shown in Figure 5, sharp crystal formation Fe 3o 4the work electrode that/rGO nano composite material is modified is than simple Fe 3o 4the work electrode modified has better response to hydrogen peroxide.Illustrate the sharp crystal formation that the present invention prepares ferromagnetic/graphene nanocomposite material has good Mimetic enzyme active, can be used for the monitoring of Small molecular hydrogen peroxide.
The explanation of above embodiment is only the preferred embodiment of the present invention; should be understood that; for the those of ordinary skill of described technical field; without departing from the inventive concept of the premise; can also carry out some improvement and modification to the present invention, these improve and modify and also should be considered as in the protection range of the claims in the present invention.

Claims (8)

1. sharp crystal formation ferromagnetic/graphene nanocomposite material, it is characterized in that, this nano composite material is by ferriferous oxide magnetic
Nano particle and Graphene are composited, ferriferous oxide magnetic nanoparticle uniform particle diameter, narrowly distributing.
2. sharp crystal formation ferromagnetic/preparation method of graphene nanocomposite material, it is characterized in that, concrete steps are as follows:
(1) first 0.03-0.3g graphene oxide is joined in the reaction unit filling 20-200mL diglycol solvent, ultrasonic 1-5h, make graphene oxide be dispersed in solvent;
(2) then, in reaction unit, add 0.12-1.2g solubility trivalent iron salt and ferrous iron magnetic metal salt stirs, under inert gas shielding, at 190-220 DEG C of temperature, add thermal agitation 0.5-2h; Wherein: described ferrous iron magnetic metal salt is Zn salt, Co salt, Ni salt, Mn salt or Cu salt;
(3) last, the 10-100mg/mLNaOH/DEG storing solution of 5-50mL is joined rapidly in said mixture, at 190-220 DEG C of temperature, reacts 1-5h, product centrifugation after washing, obtain sharp crystal formation ferromagnetic/graphene nanocomposite material.
3. preparation method according to claim 2, is characterized in that, in step (1), graphene oxide take graphite as raw material, adopts the Hummers method improved to prepare.
4. preparation method according to claim 2, is characterized in that, in step (2), the mol ratio of solubility trivalent iron salt and ferrous iron magnetic metal salt is 2:1.
5. preparation method according to claim 2, is characterized in that, in step (2), solubility trivalent iron salt is selected from Fe (NO 3) 3, FeCl 3or Fe 2(SO 4) 3in one or more.
6. preparation method according to claim 2, is characterized in that, in step (2), in ferrous iron magnetic metal salt, Zn salt is selected from ZnCl 2, ZnSO 4, Zn (NO 3) 2or Zn (CH 3cOO) 2in any one; Co salt is selected from CoCl 2, CoSO 4, Co (NO 3) 2or Co (CH 3cOO) 2in any one; Ni salt is selected from NiCl 2, NiSO 4, Ni (NO 3) 2or Ni (CH 3cOO) 2in any one; Mn salt is selected from MnCl 2, MnSO 4, Mn (NO 3) 2or Mn (CH 3cOO) 2in any one; Cu salt is selected from CuCl 2, CuSO 4, Cu (NO 3) 2or Cu (CH 3cOO) 2in any one.
7. preparation method according to claim 2, is characterized in that, in step (3); 0.2-2g NaOH is joined in 20-200mL diglycol; under inert atmosphere protection, 120-150 DEG C of temperature stirs 1-2h, is then cooled to 50-80 DEG C and makes NaOH/DEG storing solution.
8. a sharp crystal formation ferromagnetic/application of graphene nanocomposite material in Small molecular hydrogen peroxide, glucose detection.
CN201510884428.1A 2015-12-07 2015-12-07 Spinel type ferromagnet/graphene nanometer composite material, preparing method and application thereof Pending CN105513740A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107537438A (en) * 2017-08-23 2018-01-05 湖南大学 Magnetic composite nano material of graphene parcel and its preparation method and application
CN111351828A (en) * 2020-04-11 2020-06-30 石河子大学 ZnFe2O4Preparation method and application of modified electrode material

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CN101819843A (en) * 2010-03-30 2010-09-01 浙江大学 Method for preparing multifunctional graphite vinyl composite material with magnetic conductivity
US20110210282A1 (en) * 2010-02-19 2011-09-01 Mike Foley Utilizing nanoscale materials as dispersants, surfactants or stabilizing molecules, methods of making the same, and products produced therefrom
CN102745675A (en) * 2012-06-27 2012-10-24 合肥工业大学 Preparation method of spinel-type magnetic MFe2O4/graphene composite material
CN104122215A (en) * 2014-07-21 2014-10-29 济南大学 Preparation and application of regenerable photometry probe

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110210282A1 (en) * 2010-02-19 2011-09-01 Mike Foley Utilizing nanoscale materials as dispersants, surfactants or stabilizing molecules, methods of making the same, and products produced therefrom
CN101819843A (en) * 2010-03-30 2010-09-01 浙江大学 Method for preparing multifunctional graphite vinyl composite material with magnetic conductivity
CN102745675A (en) * 2012-06-27 2012-10-24 合肥工业大学 Preparation method of spinel-type magnetic MFe2O4/graphene composite material
CN104122215A (en) * 2014-07-21 2014-10-29 济南大学 Preparation and application of regenerable photometry probe

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107537438A (en) * 2017-08-23 2018-01-05 湖南大学 Magnetic composite nano material of graphene parcel and its preparation method and application
CN107537438B (en) * 2017-08-23 2020-09-04 湖南大学 Graphene-coated magnetic composite nano material and preparation method and application thereof
CN111351828A (en) * 2020-04-11 2020-06-30 石河子大学 ZnFe2O4Preparation method and application of modified electrode material

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