CN111517372A - Fullerene coated Fe3O4Composite nano material and preparation method thereof - Google Patents
Fullerene coated Fe3O4Composite nano material and preparation method thereof Download PDFInfo
- Publication number
- CN111517372A CN111517372A CN202010393567.5A CN202010393567A CN111517372A CN 111517372 A CN111517372 A CN 111517372A CN 202010393567 A CN202010393567 A CN 202010393567A CN 111517372 A CN111517372 A CN 111517372A
- Authority
- CN
- China
- Prior art keywords
- fullerene
- coated
- solution
- nano material
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical compound C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 229910003472 fullerene Inorganic materials 0.000 title claims abstract description 48
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims description 18
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 claims abstract description 39
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002131 composite material Substances 0.000 claims abstract description 27
- 239000002245 particle Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000006249 magnetic particle Substances 0.000 claims abstract description 18
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 150000003839 salts Chemical class 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 238000002425 crystallisation Methods 0.000 claims description 14
- 230000008025 crystallization Effects 0.000 claims description 14
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011258 core-shell material Substances 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 5
- -1 iron ions Chemical class 0.000 claims description 5
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 4
- 238000000975 co-precipitation Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 230000000295 complement effect Effects 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract 1
- 238000007626 photothermal therapy Methods 0.000 abstract 1
- 230000002194 synthesizing effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 49
- 239000002114 nanocomposite Substances 0.000 description 12
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 3
- 239000006247 magnetic powder Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002122 magnetic nanoparticle Substances 0.000 description 2
- 239000012266 salt solution Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910017135 Fe—O Inorganic materials 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021387 carbon allotrope Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000057 systemic toxicity Toxicity 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/08—Ferroso-ferric oxide (Fe3O4)
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/152—Fullerenes
- C01B32/154—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/42—Magnetic properties
Abstract
The invention discloses fullerene coated Fe3O4A composite nano material is prepared through improving the coprecipitation method, which includes such steps as using ferrous and ferric salts as iron source, sodium hydroxide as alkaline precipitant, and preparing Fe coated by fullerene3O4A composite nanomaterial. The method not only solves the problem of synthesizing Fe by a coprecipitation method3O4The magnetic particles are easy to agglomerate in the process, the size range is not controllable, and Fe is added3O4The fullerene particles are combined to form a coating structure, the advantages of the fullerene particles and the coating structure are complementary, the hydrophilicity of the material is improved, andthe material provides a foundation for the application in the fields of flexible sensors, photothermal therapy, biological detection and the like.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to fullerene coated Fe3O4Composite nano material and its preparation process.
Background
Ferroferric oxide belongs to one of ferric oxides and is the main component of magnetite. The ferroferric oxide magnetic powder has physicochemical properties different from those of traditional functional materials, has wider application than that of conventional magnetic materials, and is mainly applied to the fields of magnetofluid, industrial catalysis, magnetic recording materials, pharmacy, battery materials, national defense and military, micro-nano sensors and the like. The ferroferric oxide magnetic powder with the grain diameter only being nano-scale is of unprecedented concern.
The coprecipitation method is the earliest and widest application range method for preparing the ferroferric oxide magnetic powder because the method has low requirements on equipment, the reaction does not need to be carried out under the conditions of high temperature and high pressure, the reaction raw materials are cheap and easy to obtain, the process flow is simple, and the reaction process is easy to control. The coprecipitation method generally utilizes iron ions with different valence states to perform coprecipitation reaction with alkali liquor under certain conditions to generate ferroferric oxide particles, and reaction conditions such as reaction temperature and Fe are controlled3+And Fe2+Molar ratio of (2) and feed rateAnd the reaction time and the like to change the product performance, the appearance and the like.
The traditional coprecipitation method has the defects of small particle size, large specific surface area, large surface energy, unstable particles and easy agglomeration of the product nanoparticles, and is difficult to exert the characteristics of the nano material. In addition, the prepared ferroferric oxide cannot be stably dispersed in a solution due to the hydrophobicity, and can sink to the bottom of a container under the action of a gravitational field, so that the requirements of scientific research and industrial application are difficult to meet. Therefore, it is necessary to find a simple method to optimize the coprecipitation method so as to obtain magnetic nanoparticles with excellent performance and good hydrophilicity.
Fullerene (C60), a third carbon allotrope behind diamond and graphite, is a nanoscale carbon material with unique optical, electrochemical, physical properties and low systemic toxicity. The hydroxylated fullerene aqueous solution can provide a good carrier environment for inorganic materials to improve the stability of the reaction, so that Fe is added3O4The coprecipitation reaction of the particles is carried out in the hydroxylated fullerene aqueous solution, so that the performance of the product can be improved. While Fe3O4The prepared composite material can complement the advantages of fullerene, not only has good magnetic performance, but also has wave-absorbing characteristics of resistance loss, magnetic loss, dielectric loss and the like.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides fullerene coated Fe3O4The composite nano material has the advantages of good dispersibility, uniform particle size, good hydrophilicity, easily obtained reaction raw materials and simple preparation process flow.
In order to achieve the purpose, the invention is realized by the following technical scheme:
fullerene coated Fe3O4The preparation method of the composite nano material comprises the following steps:
1) dissolving hydroxylated fullerene in deionized water to prepare hydroxylated fullerene solution;
2) weighing ferrous iron salt and ferric iron salt, putting into the hydroxylated fullerene solution, and stirring for 10 minutes to fully dissolve the ferrous iron salt and the ferric iron salt;
3) slowly dropwise adding a NaOH solution into the solution obtained in the step 2) while stirring until the pH of the solution is = 12;
4) transferring the solution obtained in the step 3) to a constant-temperature water bath for crystallization reaction for a period of time;
5) absorbing the generated magnetic particles by using a magnet, and repeatedly washing the magnetic particles by using absolute ethyl alcohol and deionized water until a washing solution is neutral;
6) placing the magnetic particles obtained in the step 5) in a thermostat with the temperature of 55-65 ℃ for drying for 8-12 hours, and grinding to obtain fullerene coated Fe3O4Composite nanomaterial powder.
Preferably, the hydroxylated fullerene solution prepared in the step 1) has a hydroxylated fullerene concentration of 0.5-1 mg/ml.
Preferably, Fe is present in the solution obtained in step 2)3+And Fe2+In a molar ratio of 0.5 to 2: 1, the total concentration of iron ions in the solution is 10-20 mmol/L.
Preferably, the concentration of the NaOH solution in the step 3) is 0.1-1 mol/L.
Preferably, the temperature of the crystallization reaction in the step 4) is 50-70 ℃, and the crystallization time is 1-2 hours.
Preferably, the ferrous salt and the ferric salt are FeCl respectively2·4H2O and FeCl3·6H2O。
Fe coated with fullerene prepared by the preparation method3O4Composite nanomaterial, Fe3O4The surface of the nano-structure is wrapped by fullerene particles, and the nano-structure is of a core-shell structure, and the particle size is 15-25 nm. Fe3O4The surface contains a large amount of hydroxyl groups, and the hydrophilicity is good. The product has good dispersibility, and shows good magnetic property and superparamagnetism.
Compared with the prior art, the invention has the following beneficial effects:
the invention solves the problem of the existing preparation of high-performance Fe3O4The magnetic nano-particles have the problems of complex process and difficult control, and the provided method has simple process and high stabilityPreparation of fullerene coated Fe with good qualitative and dispersibility3O4A new technical approach to granules. Its advantages mainly include: (1) the raw materials are simple. (2) The preparation process is simple to operate. (3) And a protective agent is not required to be added, so that other substances are effectively prevented from being introduced. (4) The product has good dispersibility. (5) The product has high stability. (6) Forming fullerene coated Fe3O4And (3) a composite structure. (7) The density of the magnetic particles is reduced due to the addition of fullerene molecules. (8) Due to the hydrophilic nature of the hydroxylated fullerene, the stability of the magnetic particles in solution is improved.
Drawings
FIG. 1 shows Fe coated with fullerene obtained in example 1 of the present invention3O4TEM images of the nanocomposite particles.
FIG. 2 shows Fe coated with fullerene obtained in example 1 of the present invention3O4XRD pattern of the nanocomposite particles.
FIG. 3 shows Fe coated with fullerene obtained in example 1 of the present invention3O4FTIR plot of nanocomposite particles.
FIG. 4 shows fullerene coated Fe prepared in example 1 of the present invention3O4VSM plot of the nanocomposite particles.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments and the accompanying drawings. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solution of the present invention is described in detail below with reference to the embodiments and the drawings, but the scope of protection is not limited thereto.
Example 1
Fullerene coated Fe3O4The preparation steps of the nano composite nano material particles are as follows:
(1) 50mg of hydroxylated fullerene is taken and added with 100ml of deionized water to be stirred and dissolved to prepare hydroxylated fullerene solution.
(2) 160mgFeCl is taken2·4H2O，108mgFeCl3·6H2And O is put into the hydroxylated fullerene solution and stirred for 10 minutes to be fully dissolved.
(3) To the above solution, 0.4mol/L NaOH solution was slowly added dropwise with stirring until the pH of the solution = 12.
(4) The solution was transferred to a 50 ℃ thermostat water bath for crystallization for 1 hour.
(5) The generated magnetic particles are absorbed by a magnet and repeatedly washed by absolute ethyl alcohol and deionized water until the washing liquid is neutral.
(6) Drying in a constant temperature oven at 60 deg.C for 12 hr, and grinding to obtain fullerene/Fe with core-shell structure3O4Composite nanomaterial powder.
Example 2
Fullerene coated Fe3O4The preparation steps of the nano composite particles are as follows:
(1) 200mg of hydroxylated fullerene is taken and added with 200ml of deionized water to be stirred and dissolved to prepare a hydroxylated fullerene solution.
(2) Taking 240mgFeCl2·4H2O，324mgFeCl3·6H2And O is put into the hydroxylated fullerene solution and stirred for 10 minutes to be fully dissolved.
(3) To the above solution, a 1mol/L NaOH solution was slowly added dropwise with stirring until the pH of the solution = 12.
(4) The solution was transferred to a 60 ℃ thermostat water bath for crystallization for 1.5 hours.
(5) The generated magnetic particles are absorbed by a magnet and repeatedly washed by absolute ethyl alcohol and deionized water until the washing liquid is neutral.
(6) Drying in a thermostat at 55 deg.C for 12 hr, and grinding to obtain fullerene/Fe with core-shell structure3O4Composite nanomaterial powder.
Example 3
Fullerene coated Fe3O4The preparation method of the composite nano material comprises the following steps:
1) dissolving hydroxylated fullerene in deionized water to prepare a hydroxylated fullerene solution, wherein the concentration of the hydroxylated fullerene is 0.7 mg/ml;
2) weighing FeCl2·4H2O and FeCl3·6H2Adding O into the hydroxylated fullerene solution, stirring for 10 minutes to fully dissolve the O, and adding Fe into the solution3+And Fe2+In a molar ratio of 1: 1, the total concentration of iron ions in the solution is 15 mmol/L.
3) Slowly dropwise adding an NaOH solution into the solution obtained in the step 2) while stirring, wherein the concentration of the NaOH solution is 0.5mol/L until the pH of the solution is = 12;
4) transferring the solution obtained in the step 3) to a constant-temperature water bath for crystallization reaction for a period of time; the temperature of the crystallization reaction was 70 ℃ and the crystallization time was 1 hour.
5) Absorbing the generated magnetic particles by using a magnet, and repeatedly washing the magnetic particles by using absolute ethyl alcohol and deionized water until a washing solution is neutral;
6) placing the magnetic particles obtained in the step 5) in a thermostat at 65 ℃ for drying for 8 hours, and grinding to obtain fullerene-coated Fe with a core-shell structure3O4Composite nanomaterial powder.
Example 4
Fullerene coated Fe3O4The preparation method of the composite nano material comprises the following steps:
1) dissolving hydroxylated fullerene in deionized water to prepare a hydroxylated fullerene solution, wherein the concentration of the hydroxylated fullerene is 0.8 mg/ml;
2) weighing FeCl2·4H2O and FeCl3·6H2Adding O into the hydroxylated fullerene solution, stirring for 15 minutes to fully dissolve the O, and adding Fe into the solution3+And Fe2+In a molar ratio of 1.5: 1, the total concentration of iron ions in the solution is 12 mmol/L.
3) Slowly dropwise adding an NaOH solution into the solution obtained in the step 2) while stirring, wherein the concentration of the NaOH solution is 0.7mol/L until the pH of the solution is = 12;
4) transferring the solution obtained in the step 3) to a constant-temperature water bath for crystallization reaction; the temperature of the crystallization reaction is 55 ℃, and the crystallization time is 2 hours.
5) Absorbing the generated magnetic particles by using a magnet, and repeatedly washing the magnetic particles by using absolute ethyl alcohol and deionized water until a washing solution is neutral;
6) drying the magnetic particles obtained in the step 5) in a thermostat at 55 ℃ for 10 hours, and grinding to obtain fullerene coated Fe3O4Composite nanomaterial powder.
The method has simple operation and low equipment requirement, and does not need high-temperature and high-pressure reaction conditions. The method needs to add the hydroxylated fullerene into the solution, and has the advantages that protective gas is not needed in the reaction process, and the process flow is simpler and more convenient.
The method mixes salt solution containing ferrous ions and ferric ions according to a specific proportion, takes sodium hydroxide as an alkaline precipitator, and carries out coprecipitation reaction in hydroxylated fullerene solution to prepare fullerene coated Fe3O4A composite nanomaterial. The ferrous and ferric salt solutions can be, but are not limited to, FeCl2·4H2O and FeCl3·6H2O。
The method of the invention obtains the fullerene coated Fe3O4Composite nanomaterial, Fe3O4The surface contains a large amount of hydroxyl groups, and the product has good dispersibility, good hydrophilicity, good magnetic performance and superparamagnetism. And the fullerene is loaded on the surface of ferroferric oxide, and the size of the prepared magnetic particle is 15-25 nm. Fe3O4The surface of (a) is wrapped by fullerene particles and has a core-shell structure.
Following by TEM, XRD, FTIR, VSM for the fullerene coated Fe prepared in example 13O4Characterization of the nanocomposite particles:
TEM analysis
FIG. 1 shows fullerene-coated Fe prepared in example 13O4According to a TEM image of the nano composite particles, the product has a good dispersion effect and uniform particle size, the particle size of the product is approximately concentrated in 15-25nm, and the surface of ferroferric oxide is coated by fullerene particles. Illustrating the invention improves Fe3O4Dispersibility of particles and uniformity of particle diameterNow the fullerene is in Fe3O4And (4) coating the surface.
XRD analysis
FIG. 2 shows the fullerene coated Fe prepared in example 13O4XRD pattern of the nano composite particle, XRD diffraction peaks of the product are concentrated at 30.6 degrees, 35.8 degrees, 43.2 degrees, 57.4 degrees and 63.01 degrees, and the peaks and Fe3O4The PDF standard card (JCPDS No. 19-0629) is very consistent, and shows that after coating, Fe3O4The characteristic peak of (A) still corresponds to that of the composite material is the same as single Fe3O4Has the same structure as (1), Fe3O4The properties of (2) remain.
FTIR analysis
FIG. 3 shows FTIR spectra of the nanocomposites prepared in example 1 above. Fe3O4The corresponding spectrum of the absorption peak is 500-600cm-1Characteristic peaks of Fe-O are shown in the region. 3400cm-1The nearby wide vibration peak shows that the surface of the product contains a large number of hydroxyl groups, so that the hydrophilicity of the product is improved. At 1095, 1385 and 1622cm-1The vibrational peaks at (a) are due to the C-O, C-O-H and C-C, C = C structures present in the hydroxylated fullerene. This illustrates Fe from the side3O4Coated with fullerene.
VSM analysis
FIG. 4 shows the fullerene coated Fe prepared in example 13O4The hysteresis loop of the nano composite particles at normal temperature can be seen from the figure, the hysteresis loop of the nano composite material is a typical S-shaped curve, and the saturation magnetization can reach 69.5 emu/mg. This indicates that the present invention inherits Fe3O4Shows good magnetic properties and superparamagnetism.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. Fullerene coated Fe3O4The preparation method of the composite nano material is characterized by comprising the following steps:
1) dissolving hydroxylated fullerene in deionized water to prepare hydroxylated fullerene solution;
2) putting ferrous salt and ferric salt into the hydroxylated fullerene solution, and stirring to fully dissolve the ferrous salt and ferric salt;
3) slowly dripping NaOH solution into the solution obtained in the step 2) while stirring;
4) transferring the solution obtained in the step 3) to a constant-temperature water bath for crystallization reaction;
5) absorbing the generated magnetic particles by using a magnet, and repeatedly washing the magnetic particles by using absolute ethyl alcohol and deionized water until a washing solution is neutral;
6) placing the magnetic particles obtained in the step 5) in a constant temperature oven for drying and grinding to obtain fullerene coated Fe3O4Composite nanomaterial powder.
2. A fullerene coated Fe according to claim 13O4The preparation method of the composite nano material is characterized by comprising the following steps: the hydroxylated fullerene solution prepared in the step 1) has the concentration of 0.5-1 mg/ml.
3. A fullerene coated Fe according to claim 13O4The preparation method of the composite nano material is characterized by comprising the following steps: fe in the solution obtained in step 2)3+And Fe2+In a molar ratio of 0.5 to 2: 1, the total concentration of iron ions in the solution is 10-20 mmol/L.
4. A fullerene coated Fe according to claim 13O4The preparation method of the composite nano material is characterized by comprising the following steps: the concentration of the NaOH solution in the step 3) is 0.1-1 mol/L.
5. Such as rightFe coated with fullerene according to claim 13O4The preparation method of the composite nano material is characterized by comprising the following steps: the temperature of the crystallization reaction in the step 4) is 50-70 ℃, and the crystallization time is 1-2 hours.
6. A fullerene coated Fe according to claim 13O4The preparation method of the composite nano material is characterized by comprising the following steps: the ferrous salt and the ferric salt are FeCl respectively2·4H2O and FeCl3·6H2O。
7. A fullerene-coated Fe prepared by the method of any one of claims 1 to 63O4Composite nanomaterial characterised in that: the fullerene is coated with Fe3O4The composite nano material is of a core-shell structure, and the particle size is 15-25 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010393567.5A CN111517372A (en) | 2020-05-11 | 2020-05-11 | Fullerene coated Fe3O4Composite nano material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010393567.5A CN111517372A (en) | 2020-05-11 | 2020-05-11 | Fullerene coated Fe3O4Composite nano material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111517372A true CN111517372A (en) | 2020-08-11 |
Family
ID=71908879
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010393567.5A Pending CN111517372A (en) | 2020-05-11 | 2020-05-11 | Fullerene coated Fe3O4Composite nano material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111517372A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449343A (en) * | 2022-10-17 | 2022-12-09 | 衡阳凯新特种材料科技有限公司 | Silicon nitride wave-absorbing material and preparation method thereof |
| CN115624624A (en) * | 2022-12-22 | 2023-01-20 | 南京智正医药科技有限公司 | Application of fullerene derivative in preparation of drugs for treating alcoholic liver disease |
| CN117229820A (en) * | 2023-09-22 | 2023-12-15 | 山东海嘉石油化工有限公司 | Iron oxyhydroxide desulfurizing agent suitable for coal bed gas and preparation method thereof |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5350569A (en) * | 1993-03-30 | 1994-09-27 | The United States Of America As Represented By The United States Department Of Energy | Storage of nuclear materials by encapsulation in fullerenes |
| CN101492183A (en) * | 2009-03-05 | 2009-07-29 | 厦门大学 | Magnetic carbon nanosphere functionalized with carboxylic acid group and method of producing the same |
| US20110112232A1 (en) * | 2008-06-24 | 2011-05-12 | Vijay Krishna | Enhancement of electron scavenging by water-soluble fullerenes |
| CN102583315A (en) * | 2012-02-15 | 2012-07-18 | 西北工业大学 | Method for preparing ferroferric oxide/ carbon nano tube composite material |
| WO2012099855A2 (en) * | 2011-01-17 | 2012-07-26 | Marelle, Llc | Water-soluble functionalized fullerenes |
| US20130247993A1 (en) * | 2012-03-23 | 2013-09-26 | Xiong Gong | Enhanced Efficiency Polymer Solar Cells Using Aligned Magnetic Nanoparticles |
| CN103896247A (en) * | 2014-03-12 | 2014-07-02 | 复旦大学 | Preparation method of water-soluble fullerene nano-particles |
| CN106925298A (en) * | 2017-03-02 | 2017-07-07 | 天津大学 | A kind of fullerene/cadmium sulfide nano composite photo-catalyst and preparation method thereof |
| CN107199012A (en) * | 2017-06-12 | 2017-09-26 | 扬州工业职业技术学院 | A kind of magnetic fullerene nanomaterial and its application in SPE |
| CN108031475A (en) * | 2018-01-25 | 2018-05-15 | 太原理工大学 | A kind of preparation method of gold load ferric oxide nano photochemical catalyst |
| JP2018530513A (en) * | 2015-10-15 | 2018-10-18 | ウニベルシティ・マラヤＵｎｉｖｅｒｓｉｔｉ Ｍａｌａｙａ | Stable iron oxide magnetic nanoparticle (nanoMAG) slurry and production method thereof |
| CN109453136A (en) * | 2018-11-14 | 2019-03-12 | 山东大学 | A kind of antioxygen microcapsules and preparation method thereof containing fullerene |
-
2020
- 2020-05-11 CN CN202010393567.5A patent/CN111517372A/en active Pending
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5350569A (en) * | 1993-03-30 | 1994-09-27 | The United States Of America As Represented By The United States Department Of Energy | Storage of nuclear materials by encapsulation in fullerenes |
| US20110112232A1 (en) * | 2008-06-24 | 2011-05-12 | Vijay Krishna | Enhancement of electron scavenging by water-soluble fullerenes |
| CN101492183A (en) * | 2009-03-05 | 2009-07-29 | 厦门大学 | Magnetic carbon nanosphere functionalized with carboxylic acid group and method of producing the same |
| WO2012099855A2 (en) * | 2011-01-17 | 2012-07-26 | Marelle, Llc | Water-soluble functionalized fullerenes |
| CN102583315A (en) * | 2012-02-15 | 2012-07-18 | 西北工业大学 | Method for preparing ferroferric oxide/ carbon nano tube composite material |
| US20130247993A1 (en) * | 2012-03-23 | 2013-09-26 | Xiong Gong | Enhanced Efficiency Polymer Solar Cells Using Aligned Magnetic Nanoparticles |
| CN103896247A (en) * | 2014-03-12 | 2014-07-02 | 复旦大学 | Preparation method of water-soluble fullerene nano-particles |
| JP2018530513A (en) * | 2015-10-15 | 2018-10-18 | ウニベルシティ・マラヤＵｎｉｖｅｒｓｉｔｉ Ｍａｌａｙａ | Stable iron oxide magnetic nanoparticle (nanoMAG) slurry and production method thereof |
| CN106925298A (en) * | 2017-03-02 | 2017-07-07 | 天津大学 | A kind of fullerene/cadmium sulfide nano composite photo-catalyst and preparation method thereof |
| CN107199012A (en) * | 2017-06-12 | 2017-09-26 | 扬州工业职业技术学院 | A kind of magnetic fullerene nanomaterial and its application in SPE |
| CN108031475A (en) * | 2018-01-25 | 2018-05-15 | 太原理工大学 | A kind of preparation method of gold load ferric oxide nano photochemical catalyst |
| CN109453136A (en) * | 2018-11-14 | 2019-03-12 | 山东大学 | A kind of antioxygen microcapsules and preparation method thereof containing fullerene |
Non-Patent Citations (3)
| Title |
|---|
| MUSTAFA A. ALHEETY ET AL.: ""Eco-friendly C60-SESMP-Fe3O4 inorganic magnetizable nanocomposite as high-performance adsorbent for magnetic removal of arsenic from crude oil and water samples"", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
| 乔畅 等: ""富勒醇的制备与性能研究"", 《化工新型材料》 * |
| 陆彦峄 等: ""碳包裹对Fe3O4纳米颗粒稳定性的影响"", 《宁波大学学报（理工版）》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449343A (en) * | 2022-10-17 | 2022-12-09 | 衡阳凯新特种材料科技有限公司 | Silicon nitride wave-absorbing material and preparation method thereof |
| CN115449343B (en) * | 2022-10-17 | 2024-01-12 | 衡阳凯新特种材料科技有限公司 | Silicon nitride wave-absorbing material and preparation method thereof |
| CN115624624A (en) * | 2022-12-22 | 2023-01-20 | 南京智正医药科技有限公司 | Application of fullerene derivative in preparation of drugs for treating alcoholic liver disease |
| CN117229820A (en) * | 2023-09-22 | 2023-12-15 | 山东海嘉石油化工有限公司 | Iron oxyhydroxide desulfurizing agent suitable for coal bed gas and preparation method thereof |
| CN117229820B (en) * | 2023-09-22 | 2024-03-22 | 山东海嘉石油化工有限公司 | Iron oxyhydroxide desulfurizing agent suitable for coal bed gas and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhan et al. | Facile solvothermal preparation of Fe 3 O 4–Ag nanocomposite with excellent catalytic performance | |
| Esmaeili et al. | Modified single-phase hematite nanoparticles via a facile approach for large-scale synthesis | |
| Deng et al. | Investigation of formation of silica-coated magnetite nanoparticles via sol–gel approach | |
| CN1971780B (en) | Preparing method of nano-Fe3O4 coating carbon nanoube magnetic composite material | |
| CN111517372A (en) | Fullerene coated Fe3O4Composite nano material and preparation method thereof | |
| Zou et al. | Fe3O4 nanocrystals with novel fractal | |
| US7431862B2 (en) | Synthesis of magnetic, dielectric or phosphorescent NANO composites | |
| Zhao et al. | Hierarchically nanostructured Fe3O4 microspheres and their novel microwave electromagnetic properties | |
| CN100453220C (en) | Improved nanometer nulvalent iron particle and method for making same | |
| CN102633307A (en) | Method for hydrothermally preparing mono-dispersed hollow magnetic nanometer particles | |
| CN100355940C (en) | Method for preparing magnetic compound material of ferric oxide cladded carbon nanotube | |
| CN101728045B (en) | Cobalt oxide/carbon composite nano wave-absorbing material and preparation method thereof | |
| CN109665565B (en) | Nano Fe3O4Preparation method of composite graphene and nano Fe3O4Composite graphene | |
| CN100344708C (en) | Method for preparing carbon nanotube magnetic compositematerial modified by iron oxide red | |
| CN104722777A (en) | Quick preparation method for starch-stabilizing nanometer zero-valent iron | |
| CN100453469C (en) | Method for preparing Nano cube of hematite | |
| CN101125684A (en) | Preparation method for gamma-Fe2O3 magnetic nano particles | |
| CN101786601B (en) | Preparation method of compound nano particle with Fe3O4/CoO core shell structure | |
| CN102001712A (en) | Method for preparing superparamagnetic Fe3O4 nano particle based on thermal decomposition of template | |
| Antarnusa et al. | The effect of additional polyethylene glycol (PEG) as coating Fe3O4 for magnetic nanofluid applications | |
| CN1230472C (en) | Method for preparing nano iron oxide red | |
| Li et al. | Analysis of the factors affecting the magnetic characteristics of nano-Fe 3 O 4 particles | |
| Tago et al. | Preparation and properties of silica-coated metallic nickel particles | |
| CN101962210A (en) | Industrialized preparation method for monodisperse cobalt ferrite nanoparticles | |
| CN108971509A (en) | A kind of preparation method of the iron-nickel alloy nano material of controllable grain size |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200811 |