CN107537438A - Magnetic composite nano material of graphene parcel and its preparation method and application - Google Patents
Magnetic composite nano material of graphene parcel and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of magnetic composite nano material and its preparation method and application of graphene parcel, the magnetic composite nano material be by shell of graphene, gold cobalt alloy be core shell structure that core forms, the graphene is directly wrapped in the surface of gold cobalt alloy；Magnetic composite nano material is graininess, and particle diameter is 20 40 nm.Preparation method of the present invention is simple, and cost is low, and controllability is strong, and the MACGs composite nanometer particles homogeneity prepared is good, and property is stable.
Description
Technical field
The present invention relates to magnetic composite nano material of graphene parcel and its preparation method and application, belong to novel magnetic
The technical field of composite nano materials.
Background technology
Composite nano materials are research topics more popular at present, due to it with multi-functional, coordinability and surely
It is qualitative to wait good characteristic, it is had in fields such as optics, biomedicine, environmental science, material, catalysis, the energy very extensive
Application.Compared with monocomponent nanocomposite material, multicomponent composite nano materials are made it have by regulating and controlling its composition or structure
More excellent property, this has also expanded its application potential in multiple fields.Recently, magnetic composite nano material is due to its magnetic
Property and stability widely paid close attention to, thus prepare size uniformity, stably, be easy to modification, good biocompatibility
Magnetic composite nano material in biological concentration, separation and other research fields for all having very important application value.
It is by Fe to prepare a kind of method of magnetic composite nano material at present3O4Formed with AuNPs by covalently bound mode
The core-shell nano material of magnetic, another method are in Fe3O4Nano grain surface wraps by way of gold reduces on its surface
Wrap up in golden shell layer, be synthetic method complexity, size heterogeneity, the in addition stability of material and life the shortcomings that above both approaches
Thing compatibility is also bad, and which limits its application in field of bioanalysis.
The content of the invention
Present invention solves the technical problem that being, the synthetic method of magnetic composite nano material is complicated at present, size heterogeneity,
In addition the stability of material and biocompatibility are also bad, and which limits its application in field of bioanalysis.
The present invention provides a kind of magnetic composite nano material of graphene parcel, and the magnetic composite nano material is with graphite
The core shell structure that alkene is shell, gold cobalt alloy is core composition, the graphene are directly wrapped in the surface of gold cobalt alloy；Magnetic coupling
Nano material is graininess, particle diameter 20-40nm.
Preferably, the number of plies of the graphene on gold cobalt alloy surface is 3-4 layers.
Preferably, the middle gold of gold cobalt alloy and the mol ratio of cobalt are 8:1-1:1.
Preferably, the middle gold of gold cobalt alloy and the mol ratio of cobalt are 7:1-5:1.
The present invention also provides a kind of preparation method of the magnetic composite nano material of graphene parcel, comprises the following steps：
（1）By SiO2Add and 1-2 h are ultrasonically treated in methanol solution, obtain solution A, wherein, SiO2With the mass volume ratio of methanol
For 1:80-100, mass unit g, volume unit mL；By Co (NO3)2·6H2O and 5-20 mg/mL HAuCl4Solution mixes
After conjunction, solution B is obtained；Carry out being ultrasonically treated 1-2 h after the solution B of the solution A of 40-60 parts by volume and 1 parts by volume is mixed, then remove
Methanol is removed, obtained mixture is dried；
（2）By step（1）The mixture grind into powder of drying, then in CH4Flow is 10-60 cm2/ mL flow conditions
Lower calcination 10-15 min, calcination temperature are 800-1000 DEG C, are mixed after cooling with HF solution to remove SiO2, then separate（It is excellent
Magnetic is selected to separate）The solid gone out is the magnetic composite nano particle of graphene parcel.
Preferably, step（2）In, the mass volume ratio of powder and HF solution is 0.75-0.85:25-30, mass unit are
G, mass fraction >=40% of volume unit mL, HF solution.The mass fraction of HF solution is 40-60%.
Preferably, step（1）Described in the power of ultrasonication be 170-200 w.
Preferably, step（1）In, Au and Co mol ratio is 10 in solution B:1-1:2.
Preferably, by step（2）In obtain graphene parcel magnetic composite nano material be scattered in polyethylene glycol 18
In the aqueous solution of ether, the preferred saturated aqueous solution of the ether of polyethylene glycol 18, the magnetic composite nano particle of graphene parcel is obtained
Solution.
Preferably, the magnetic composite nano material or above-mentioned magnetic composite nano material that above-mentioned preparation method obtains are in life
Application in thing imaging.
The present invention have developed a kind of magnetic composite nano material of novel graphite alkene parcel（Magnetic AuCo@
graphene, MACGs）, the alloy that the core of the material is formed by gold and two kinds of metallic elements of cobalt forms, makes material while have
The property being magnetic with plasma, the graphene that golden cobalt nano-particle surface is uniformly wrapped up in addition make that material is more stable, is easy to
Modification, good biocompatibility.Gold nano grain can be used as SERS in MACGs composite nano materials
（Surface-Enhanced Raman Scattering, SERS）Substrate, the highly sensitive detection for Raman signal molecule.
The graphene of MACGs surfaces parcel has unique Raman scattering peak, available for SERS Raman images.In addition MACGs is compound receives
The magnetic property of rice material makes it in magnetic resonance imaging（Magnetic Resonance Imaging, MRI）And in terms of magnetic enrichment
Also there is good application potential.
The method operating procedure used in MACGs composite nano materials that the present invention synthesizes is simple, the scantling of synthesis is equal
One, and the graphene for being wrapped in material surface not only increases the biocompatibility of material, and it is easier to material surface
Modification, makes it all have good application value in multiple fields.
Compared with prior art, beneficial effects of the present invention are：Preparation method of the present invention is simple, and cost is low, and controllability is strong.
The MACGs composite nanometer particles homogeneity prepared is good, and property is stable.And this composite nanometer particle has a variety of properties, makes
Its biological detection, two-photon fluorescence and computerized tomography under Raman enhancing, magnetic resonance imaging, magnetic enrichment, extreme condition
The fields such as scanning imagery all have good application prospect.The graphene that MACGs nano grain surfaces uniformly wrap up, make material more
Stabilization, it is easy to modification, good biocompatibility.Gold nano grain can be used as SERS substrates in MACGs composite nano materials, for drawing
The highly sensitive detection of graceful signaling molecule.The graphene of MACGs surfaces parcel has unique Raman scattering peak, is drawn available for SERS
Graceful imaging.In addition, the magnetic property of MACGs composite nano materials makes it also have well in terms of MRI imagings and magnetic enrichment
Application value.
Brief description of the drawings
Fig. 1 is the phenogram of MACGs nano particles prepared by the present invention；Wherein, a）For MACGs schematic diagram, b）For
MACGs UV-visible absorption spectrum, c）And d) be MACGs transmission electron microscope picture, d) in interior illustration be Au, Co alloy
Lattice fringe figure, e) be MACGs scanning transmission electron microscope figure（It is left：Dark-field imaging；In：Au；It is right：Co）；
Fig. 2 is the Raman spectrogram and Raman image figure of MACGs nano particles prepared by the present invention；Wherein, a）For MACGs drawing
Graceful spectrogram, b）For R6G Raman enhanced spectrum figure, c）For the Raman image figure (imaging of G peaks) of nematode；
Fig. 3 is MRI imagings and the concentration effect figure of MACGs nano particles prepared by the present invention；a）For MACGs T2Relaxation value,
b）For MACGs MRI images, c）To be enriched with the signal intensity figure of front and rear Raman signal molecule with MACGs.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
The preparation method of the magnetic composite nano material of graphene parcel comprises the following steps：
（1）Weigh 3.0 g SiO2, supersound process 1-2 h in 240 mL methanol solutions are added into, obtain solution A；Weigh 6.0
Mg Co (NO3)2· 6H2O and the mg/mL of 5.0 mL 10 HAuCl4After mixing（Au and Co mol ratio is 6:1）, obtain molten
Liquid B；Carry out being ultrasonically treated 1-2 h again after mixing solution A and B solution, methanol is removed, by obtained mixture in 45-50 DEG C of bar
Dried under part；Wherein, step（1）Described in be ultrasonically treated refer to be ultrasonically treated under the conditions of 200 w；
（2）By step（1）After the mixture drying of gained, grind into powder, then in CH4Flow is 10 cm2/ mL air-flow
Under the conditions of the min of calcination 13, calcination temperature be 1000 DEG C, mix after cooling with HF solution, magnetic removing HF solution after obtain stone
The magnetic composite nano particle of black alkene parcel；Wherein, the mass volume ratio of powder and HF solution is 0.75-0.85:25-30, matter
Amount unit is g, volume unit mL.
Embodiment 2
The preparation method of the magnetic composite nano material of graphene parcel comprises the following steps：
（1）Weigh 3.0 g SiO2, it is added into 240 mL methanol solutions and is ultrasonically treated 1.5 h, obtains solution A；Weigh 6.0
Mg Co (NO3)2· 6H2O and the mg/mL of 5.0 mL 10 HAuCl4After mixing, solution B is obtained；After mixing solution A and B solution
Carry out being ultrasonically treated 1.5 h again, remove methanol, obtained mixture is dried under the conditions of 45-50 DEG C；The work(of supersound process
Rate is 200 w；
（2）By step（1）After the mixture drying of gained, grind into powder, then in CH4Flow is 60 cm2/ mL air-flow
Under the conditions of the min of calcination 13, calcination temperature be 1000 DEG C, mix after cooling with HF solution, magnetic removing HF solution after obtain stone
The magnetic composite nano particle of black alkene parcel；Wherein, the mass volume ratio of powder and HF solution is 0.75-0.85:25-30, matter
Amount unit is g, volume unit mL.
（3）By step（2）The magnetic composite nano particle of graphene parcel and the C of saturation of collection18- PEG (polyethylene glycol
18 ethers, C18H37(OCH2CH2)nOH, n are about 100, are bought in SIGMA-ALDRICH, No. CAS：9005-00-9) aqueous solution is pressed
Mass volume ratio 13.9-14.5:15-20 is mixed, and mass unit mg, volume unit is μ L, is ultrasonically treated under the conditions of 200 w
1-2 h, are completely dissolved to particle, produce the magnetic composite nano material solution of stable graphene parcel.
As shown in Figure 1, the MACGs size uniformities of synthesis, particle diameter are about 30 nm or so（Fig. 1 c）, particle surface is uniform
Wrap up 3-4 layer graphenes（Fig. 1 d）, from Fig. 1 e, MACGs core is made up of the alloy of two kinds of elements of Au and Co.By scheming
2 understand, the graphene of MACGs surfaces parcel has unique Raman scattering peak（D, G, 2D peak）（Fig. 2 a）, unique using it
Raman scattering peak（G peaks）Available for biosystem（Nematode）Imaging（Fig. 2 c）, in addition, MACGs can also be used for Raman enhancing base
Bottom is used for Raman signal molecule（R6G）Enhancing（Fig. 2 b）.From the figure 3, it may be seen that MACGs is a kind of T2Contrast agent（Fig. 3 a）, Fig. 3
B is the magnetic resonance imaging figure under the corresponding MACGs concentration of Fig. 3 a, illustrates that MACGs can be used as T2Contrast agent is used in biosystem
Magnetic resonance imaging, also with MACGs magnetic, available for the enrichment of biomolecule, Fig. 3 c are the Raman letter under various concentrations
Number molecule is under MACGs enrichment, the enhancing of Raman signal intensity.Analyzed more than, synthesized by this invention
The magnetic composite nano material of graphene parcel has the following advantages that：1. synthesis step is simple, size uniformity, good properties；2.
MACGs nano particles can be used as a kind of Raman enhancing substrate, the highly sensitive detection for Raman signal molecule；3. itself
Raman scattering property with uniqueness, available for SERS Raman images；4. MACGs nano materials are a kind of T2Contrast agent, it can use
It is imaged in MRI；5. using the magnetic property of MACGs nano materials in itself, under conditions of externally-applied magnetic field, biomolecule can be achieved
Separation and enrichment.6. in addition, MACGs nano particles also have in the field such as two-photon fluorescence and Computed tomography
Good application prospect.
Embodiment 3
Experimental procedure is same as Example 1, and difference is and has investigated other CH4Flow（20, 30, 40, 50 cm2/mL）
Influence to synthesized MACGs patterns, from experimental result, in the range of the methane flow investigated, to synthesized
The influence of MACGs patterns is simultaneously little, so the flow of last optimization methane is 40 cm2/mL。
Embodiment 4
Experimental procedure is same as Example 1, and difference is that the flow of methane is 40 cm2/ mL, Co (NO3)2· 6H2O quality
For 20.3 mg, HAuCl4（10 mg/mL）Volume be 2.9 mL（Au and Co mol ratio is 1:1）, synthesized under the conditions of this
The graphene of MACGs particle surfaces parcel is uneven, and has the generation of substantial amounts of indefinite form carbon.
Claims (10)
1. a kind of magnetic composite nano material of graphene parcel, it is characterised in that the magnetic composite nano material is with graphite
The core shell structure that alkene is shell, gold cobalt alloy is core composition, the graphene are directly wrapped in the surface of gold cobalt alloy；Magnetic coupling
Nano material is graininess, and particle diameter is 20-40 nm.
2. magnetic composite nano material as claimed in claim 1, it is characterised in that the number of plies of the graphene on gold cobalt alloy surface
For 3-4 layers.
3. magnetic composite nano material as claimed in claim 1, it is characterised in that the mol ratio of the middle gold and cobalt of gold cobalt alloy
For 8:1-1:1.
4. magnetic composite nano material as claimed in claim 1, it is characterised in that the mol ratio of the middle gold and cobalt of gold cobalt alloy
For 7:1-5:1.
5. a kind of preparation method of the magnetic composite nano material of the graphene parcel described in any one of claim 1-4, it is special
Sign is, comprises the following steps：
（1）By SiO2Add and 1-2 h are ultrasonically treated in methanol solution, obtain solution A, wherein, SiO2Mass volume ratio with methanol is
1:80-100, mass unit g, volume unit mL；By Co (NO3)2·6H2O and 5-20 mg/mL HAuCl4Solution mixes
After conjunction, solution B is obtained；Carry out being ultrasonically treated 1-2 h after the solution B of the solution A of 40-60 parts by volume and 1 parts by volume is mixed, then remove
Methanol is removed, obtained mixture is dried；
（2）By step（1）The mixture grind into powder of drying, then in CH4Flow is 10-60 cm2Under/mL flow conditions
Calcination 10-15 min, calcination temperature are 800-1000 DEG C, are mixed after cooling with HF solution, then isolate the solid in solution,
The as magnetic composite nano particle of graphene parcel.
6. preparation method as claimed in claim 5, it is characterised in that step（2）In, the mass volume ratio of powder and HF solution
For 0.75-0.85:25-30, mass unit g, the % of the mass fraction of volume unit mL, HF solution >=40.0.
7. preparation method as claimed in claim 5, it is characterised in that step（1）Described in the power of ultrasonication be
170-200 w。
8. preparation method as claimed in claim 5, it is characterised in that step（1）In, Au and Co mol ratio is in solution B
10:1-1:2。
9. preparation method as claimed in claim 5, it is characterised in that by step（2）In obtain graphene parcel magnetic answer
Close nano material to be scattered in the aqueous solution of the ether of polyethylene glycol 18, the magnetic composite nano particle for obtaining graphene parcel is molten
Liquid.
10. the magnetic composite nano material described in claim any one of 1-4, or the preparation described in claim any one of 5-9
Application of the magnetic composite nano material that method obtains in bio-imaging.
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| CN108426870A (en) * | 2018-04-26 | 2018-08-21 | 湖南大学 | A kind of surface enhanced Raman scattering substrate and preparation method thereof |
| CN110567940A (en) * | 2019-11-06 | 2019-12-13 | 滨州医学院 | Silver-coated gold SERS substrate and preparation method thereof |
| CN111005091A (en) * | 2019-12-30 | 2020-04-14 | 西北工业大学 | Preparation method of high-stability flexible graphene/AuNPs SERS substrate composite fiber |
| CN113020590A (en) * | 2021-03-02 | 2021-06-25 | 湖南大学 | Graphene-coated cobalt-platinum composite nano material and preparation process and application thereof |
| CN114023561A (en) * | 2021-10-29 | 2022-02-08 | 华中科技大学 | Extrinsic two-dimensional composite magnetic material, preparation method and application |
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| CN114023561A (en) * | 2021-10-29 | 2022-02-08 | 华中科技大学 | Extrinsic two-dimensional composite magnetic material, preparation method and application |
| CN114023561B (en) * | 2021-10-29 | 2022-12-09 | 华中科技大学 | Extrinsic two-dimensional composite magnetic material, preparation method and application |
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