CN111777063A - Preparation method of nano material - Google Patents
Preparation method of nano material Download PDFInfo
- Publication number
- CN111777063A CN111777063A CN202010656427.2A CN202010656427A CN111777063A CN 111777063 A CN111777063 A CN 111777063A CN 202010656427 A CN202010656427 A CN 202010656427A CN 111777063 A CN111777063 A CN 111777063A
- Authority
- CN
- China
- Prior art keywords
- graphene
- ferrite
- ethanol
- stirring
- volume
- 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
Images
Classifications
-
- 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
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- 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
- 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)
-
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
A preparation method of a nano material comprises the steps of respectively dissolving ferrite and graphene in an ethanol solution; then uniformly mixing the two obtained solutions, performing ultrasonic stirring and vacuum filtration treatment to obtain a solid substance containing ferrite, graphene and ethanol; then putting the solid substance into a vacuum oven for drying to obtain a nano material containing ferrite and graphene; the invention can prepare the nano material with stable structure.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method of a nano material.
Background
The nano material is a micro-structure powder material prepared by powder with the particle size on the nano scale through a certain process means, has the advantages of large specific surface area, high specific strength, excellent electromagnetic property and the like due to smaller particle size, and is widely applied to the fields of material filling modification, electromagnetic wave absorption, precise sensing, catalytic reaction and the like.
Many nanomaterials with complex structures have been reported, and for most nanomaterials their properties are closely related to their unique structures. However, the preparation methods of nano materials at home and abroad are relatively traditional, mainly including chemical grafting reaction, vapor deposition, liquid phase blending, hydrothermal method and the like, and obviously, the small-batch production, high cost and complex process of the methods hinder the industrial application of the nano materials. The preparation of nanomaterials with structural properties requires a more simple and flexible process, the mechanical blending process allows the manufacture of nanomaterials with certain structural properties, and the simplicity, large-scale, low production cost are significant advantages of this process.
In the field of preparing nano materials by a mechanical blending method, the prior art only realizes simple compounding of different nano materials, the structural stability of the compounded nano material is not high, the structure of the nano material is often easily damaged by the mechanical action of the external environment, and the application of the nano material in engineering is not facilitated.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a nano material, which can be used for preparing a graphene @ ferroferric oxide nano material with a stable structure.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a nano material comprises the following steps:
1) pouring ferrite into ethanol with a first volume, and mixing and stirring to obtain an ethanol solution containing the ferrite;
2) pouring graphene into ethanol with a second volume, mixing and stirring to obtain an ethanol solution containing graphene;
3) adding the ethanol solution containing graphene into the ethanol solution containing ferrite through a separating funnel, performing ultrasonic stirring and vacuum filtration to obtain a solid matter, wherein the solid matter contains ferrite, graphene and ethanol;
4) and (3) putting the solid substance into a vacuum oven for drying treatment to obtain the nano material containing ferrite and graphene.
The first capacity in the step 1) is 200-400 g; and pouring the ferrite into ethanol with the first volume for mixing and stirring for 15-30 minutes, wherein the volume of the ferrite is 5-15 g. The second capacity in the step 2) is 450-750 g; and pouring the graphene into the ethanol with the second volume, mixing and stirring for 5-10 minutes, wherein the volume of the graphene is 5-10 g. The volume ratio of the ferrite in the step 1) to the graphene in the step 2) is 1-3: 1-2.
The ultrasonic stirring and vacuum filtration process in the step 3) comprises the following steps: ultrasonic treatment is carried out by adopting ultrasonic equipment with the ultrasonic frequency of 6.5 kHz; uniformly stirring the liquid after ultrasonic treatment by adopting a stirrer with the rotating speed of 650 rpm; carrying out suction filtration treatment on the liquid obtained after the stirring treatment by using vacuum filtration equipment; wherein the stirring time is 10-25 minutes; the vacuum filtration time is at least 12 hours.
The drying temperature of the vacuum oven in the step 4) is 45 degrees; the drying time is at least 18 hours.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. the preparation method of the graphene @ ferroferric oxide nano material with the interlayer structure by the mechanical blending method is different from the traditional preparation method, the opening of the graphene lamellar structure, the embedding of the ferroferric oxide nano material and the closing integration of the graphene lamellar structure are realized by the technical means, the whole preparation process does not need high temperature and high pressure, precise manufacturing equipment is not needed, the mass and quick manufacturing of the nano material can be realized, and the product development period is greatly shortened.
2. The invention solves the problem of poor stability of the nano powder prepared by the traditional mechanical blending method, particularly on the interface stability between ferroferric oxide and graphene; when ferroferric oxide is embedded into the opened graphene sheet layer material, the graphene sheet layer is closed under the action of free aggregation of graphene and vacuum pressure of suction filtration equipment, and the closure of the graphene sheet layer is the closure of molecular force between pi-pi bonds, so that the stability of the nano material is greatly improved.
Drawings
FIG. 1 shows the xrd, sem and magnetic field absorption patterns of the nanomaterials obtained in example 1.
FIG. 2 is the xrd, sem and magnetic field absorption diagrams of the nanomaterials obtained in example 2.
FIG. 3 shows the xrd, sem and magnetic field absorption diagrams of the nanomaterials obtained in example 3.
Detailed Description
The process of the present invention will be described in detail with reference to examples.
1) 5.0000g of ferrite powder is weighed by an analytical balance, added into 300g of ethanol solution and uniformly stirred for 15 minutes by a stirrer with the rotating speed of 650rpm to obtain ethanol solution containing ferrite;
2) 5.0000g of graphene powder is weighed by an analytical balance, added into 450g of ethanol solution, and uniformly stirred for 5 minutes by a stirrer with the rotating speed of 650rpm to obtain ethanol solution containing graphene;
3) dropwise adding the ethanol solution containing graphene into the ethanol solution containing ferrite through a separating funnel, and performing ultrasonic treatment by adopting ultrasonic equipment with ultrasonic frequency of 6.5 kHz; uniformly stirring the liquid after ultrasonic treatment for 10 minutes by adopting a stirrer with the rotating speed of 650 rpm; carrying out suction filtration treatment on the liquid obtained after the stirring treatment for 12 hours by using vacuum filtration equipment; obtaining a solid substance containing ferrite, graphene and ethanol;
4) in order to sufficiently disperse ethanol in the solid substance obtained in the step 3), so as to reduce the influence of ethanol liquid on the structure of the nano material; putting a solid matter containing ferrite, graphene and ethanol into a vacuum oven, setting the temperature of the oven at 45 ℃ and the drying time at 18 hours, and performing drying operation; and fully dispersing the ethanol to obtain the nano material containing the ferrite and the graphene.
The beneficial effect of this embodiment does: xrd and sem tests of the nanomaterial prepared in the embodiment show that the ferrite is successfully embedded into the graphene sheet layer, and the prepared nanomaterial is placed in an alcohol solution for magnetic adsorption to find that the nanomaterial is successfully adsorbed on one side, which indicates that the stable nanomaterial is prepared.
1) 15.0000g of ferrite powder is weighed by an analytical balance, added into 400g of ethanol solution and uniformly stirred for 30 minutes by a stirrer with the rotating speed of 650rpm to obtain ethanol solution containing ferrite;
2) 5.0000g of graphene powder is weighed by an analytical balance, added into 600g of ethanol solution, and uniformly stirred for 5 minutes by a stirrer with the rotating speed of 650rpm to obtain ethanol solution containing graphene;
3) dropwise adding the ethanol solution containing graphene into the ethanol solution containing ferrite through a separating funnel, and performing ultrasonic treatment by adopting ultrasonic equipment with ultrasonic frequency of 6.5 kHz; uniformly stirring the liquid after ultrasonic treatment for 15 minutes by adopting a stirrer with the rotating speed of 650 rpm; carrying out suction filtration treatment on the liquid obtained after the stirring treatment for 12 hours by using vacuum filtration equipment; obtaining a solid substance containing ferrite, graphene and ethanol;
4) in order to sufficiently disperse ethanol in the solid substance obtained in the step 3), so as to reduce the influence of ethanol liquid on the structure of the nano material; putting a solid matter containing ferrite, graphene and ethanol into a vacuum oven, setting the temperature of the oven at 45 ℃ and the drying time at 18 hours, and performing drying operation; and fully dispersing the ethanol to obtain the nano material containing the ferrite and the graphene.
The beneficial effect of this embodiment does: xrd and sem tests of the nanomaterial prepared in the embodiment show that the ferrite is successfully embedded into the graphene sheet layer, and the prepared nanomaterial is placed in an alcohol solution for magnetic adsorption to find that the nanomaterial is successfully adsorbed on one side, which indicates that the stable nanomaterial is prepared.
1) 5.0000g of ferrite powder is weighed by an analytical balance, added into 200g of ethanol solution and uniformly stirred for 15 minutes by a stirrer with the rotation speed of 650rpm to obtain ethanol solution containing ferrite;
2) weighing 10.0000g of graphene powder by using an analytical balance, adding the graphene powder into 750g of ethanol solution, and uniformly stirring for 10 minutes by using a stirrer with the rotating speed of 650rpm to obtain ethanol solution containing graphene;
3) dropwise adding the ethanol solution containing graphene into the ethanol solution containing ferrite through a separating funnel, and performing ultrasonic treatment by adopting ultrasonic equipment with ultrasonic frequency of 6.5 kHz; uniformly stirring the liquid after ultrasonic treatment for 25 minutes by adopting a stirrer with the rotating speed of 650 rpm; carrying out suction filtration treatment on the liquid obtained after the stirring treatment for 12 hours by using vacuum filtration equipment; obtaining a solid substance containing ferrite, graphene and ethanol;
4) in order to sufficiently disperse ethanol in the solid substance obtained in the step 3), so as to reduce the influence of ethanol liquid on the structure of the nano material; putting a solid matter containing ferrite, graphene and ethanol into a vacuum oven, setting the temperature of the oven at 45 ℃ and the drying time at 18 hours, and performing drying operation; and fully dispersing the ethanol to obtain the nano material containing the ferrite and the graphene.
The beneficial effect of this embodiment does: xrd and sem tests of the nanomaterial prepared in the embodiment show that the ferrite is successfully embedded into the graphene sheet layer, and the prepared nanomaterial is placed in an alcohol solution for magnetic adsorption to find that the nanomaterial is successfully adsorbed to one side, which indicates that the stable nanomaterial is prepared.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can substitute or change the technical solution of the present invention and the inventive concept within the technical scope of the present invention, and the technical solution and the inventive concept thereof should be covered by the present invention.
Claims (6)
1. The preparation method of the nano material is characterized by comprising the following steps of:
1) pouring ferrite into ethanol with a first volume, and mixing and stirring to obtain an ethanol solution containing the ferrite;
2) pouring graphene into ethanol with a second volume, mixing and stirring to obtain an ethanol solution containing graphene;
3) adding the ethanol solution containing graphene into the ethanol solution containing ferrite through a separating funnel, performing ultrasonic stirring and vacuum filtration to obtain a solid matter, wherein the solid matter contains ferrite, graphene and ethanol;
4) and (3) putting the solid substance into a vacuum oven for drying treatment to obtain the nano material containing ferrite and graphene.
2. The method for preparing nano-materials according to claim 1, wherein: the first capacity in the step 1) is 200-400 g; and pouring the ferrite into ethanol with the first volume for mixing and stirring for 15-30 minutes, wherein the volume of the ferrite is 5-15 g.
3. The method for preparing nano-materials according to claim 1, wherein: the second capacity in the step 2) is 450-750 g; and pouring the graphene into the ethanol with the second volume, mixing and stirring for 5-10 minutes, wherein the volume of the graphene is 5-10 g.
4. The method for preparing nano-materials according to claim 1, wherein: the volume ratio of the ferrite in the step 1) to the graphene in the step 2) is 1-3: 1-2.
5. The method for preparing nano-materials according to claim 1, wherein the ultrasonic agitation and vacuum filtration process in step 3) comprises: ultrasonic treatment is carried out by adopting ultrasonic equipment with the ultrasonic frequency of 6.5 kHz; uniformly stirring the liquid after ultrasonic treatment by adopting a stirrer with the rotating speed of 650 rpm; carrying out suction filtration treatment on the liquid obtained after the stirring treatment by using vacuum filtration equipment; wherein the stirring time is 10-25 minutes; the vacuum filtration time is at least 12 hours.
6. The method for preparing nano-materials according to claim 1, wherein: the drying temperature of the vacuum oven in the step 4) is 45 degrees; the drying time is at least 18 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010656427.2A CN111777063A (en) | 2020-07-09 | 2020-07-09 | Preparation method of nano material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010656427.2A CN111777063A (en) | 2020-07-09 | 2020-07-09 | Preparation method of nano material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111777063A true CN111777063A (en) | 2020-10-16 |
Family
ID=72759414
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010656427.2A Pending CN111777063A (en) | 2020-07-09 | 2020-07-09 | Preparation method of nano material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111777063A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833032A (en) * | 2014-03-11 | 2014-06-04 | 中国第一汽车股份有限公司 | Graphene-based composite cathode material |
| CN105879880A (en) * | 2016-04-25 | 2016-08-24 | 江苏大学 | Composite nano material and preparation method thereof and application |
| CN106211728A (en) * | 2016-07-10 | 2016-12-07 | 上海大学 | A kind of graphene coated Fe3o4the composite wave-suction material preparation method of nano-particle |
| US20170136062A1 (en) * | 2015-11-17 | 2017-05-18 | Alfaisal University | Method of making nanocomposites of metal oxide and reduced graphene oxide and use for cancer treatment |
| CN106925296A (en) * | 2017-03-28 | 2017-07-07 | 青岛科技大学 | A kind of nano composite material and its preparation method and application |
| CN107649113A (en) * | 2017-10-23 | 2018-02-02 | 南京旭羽睿材料科技有限公司 | A kind of catalyst with graphene oxide |
| CN108249482A (en) * | 2017-12-28 | 2018-07-06 | 杭州电子科技大学 | Magnetic Fe2O3The preparation method of nano particle and its method compound with nano-carbon material |
-
2020
- 2020-07-09 CN CN202010656427.2A patent/CN111777063A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103833032A (en) * | 2014-03-11 | 2014-06-04 | 中国第一汽车股份有限公司 | Graphene-based composite cathode material |
| US20170136062A1 (en) * | 2015-11-17 | 2017-05-18 | Alfaisal University | Method of making nanocomposites of metal oxide and reduced graphene oxide and use for cancer treatment |
| CN105879880A (en) * | 2016-04-25 | 2016-08-24 | 江苏大学 | Composite nano material and preparation method thereof and application |
| CN106211728A (en) * | 2016-07-10 | 2016-12-07 | 上海大学 | A kind of graphene coated Fe3o4the composite wave-suction material preparation method of nano-particle |
| CN106925296A (en) * | 2017-03-28 | 2017-07-07 | 青岛科技大学 | A kind of nano composite material and its preparation method and application |
| CN107649113A (en) * | 2017-10-23 | 2018-02-02 | 南京旭羽睿材料科技有限公司 | A kind of catalyst with graphene oxide |
| CN108249482A (en) * | 2017-12-28 | 2018-07-06 | 杭州电子科技大学 | Magnetic Fe2O3The preparation method of nano particle and its method compound with nano-carbon material |
Non-Patent Citations (1)
| Title |
|---|
| JISHENG ZHOU ET AL.: "Magnetite/grapheme nanosheet composites: interfacial interaction and its impact on the durable high-rate performance in lithium-ion batteries", 《RSC ADVANCES》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wang et al. | Biomass carbon derived from pine nut shells decorated with NiO nanoflakes for enhanced microwave absorption properties | |
| CN104610913B (en) | A kind of preparation method of the microwave absorbing material with MOFs molecular structure as template | |
| Jain et al. | Structural studies of lithium intercalation in a nanocrystalline α-Fe2O3 compound | |
| WO2015139517A1 (en) | Barrier anti-static tpu composite material film and preparation method therefor | |
| Tao et al. | Fabrication of nickel hydroxide microtubes with micro-and nano-scale composite structure and improving electrochemical performance | |
| CN109825252B (en) | Core-shell structure Fe3O4@C@MoS2Preparation of composite material and application thereof | |
| CN106975489B (en) | Preparation method of nickel oxide in-situ coated graphene nanocomposite | |
| CN103613755A (en) | Graphene/polyaniline nanometer composite material, preparation method and application | |
| CN107486135B (en) | Bentonite-coated ferroferric oxide nano material and preparation method and application thereof | |
| CN106328336B (en) | A kind of preparation method of the magnetic carbon nano-tube based on charge effect | |
| Jiao et al. | Self-assembly of biosurfactant–inorganic hybrid nanoflowers as efficient catalysts for degradation of cationic dyes | |
| Lan et al. | Sesbania gum-based magnetic carbonaceous nanocomposites: Facile fabrication and adsorption behavior | |
| Tang et al. | Ni-Co layered double hydroxide nanosheet array on nickel foam coated graphene for high-performance asymmetric supercapacitors | |
| CN111574667A (en) | High-strength carbon nanotube grafted modified polystyrene dielectric material and preparation method thereof | |
| CN110665465A (en) | Magnetic covalent organic framework material for glycopeptide enrichment and preparation method and application thereof | |
| Sun et al. | Early hydration properties of Portland cement with lab-synthetic calcined stöber nano-SiO2 particles as modifier | |
| CN105397106A (en) | Method of preparing nanoscale zero-valent iron particles through improved liquid phase reduction method | |
| Zhao et al. | Polyurethane sponge-derived nitrogen-doped carbon-encapsulation composite for enhanced lithium-ion battery performances | |
| Lin et al. | Polypyrrole nanotube/ferrocene-modified graphene oxide composites: From fabrication to EMI shielding application | |
| Guo et al. | Improved electrocatalytic performance from graphene quantum dots/three-dimensional graphene/polyaniline doped powder to layer-by-layer self-assembled membrane materials | |
| CN103028738B (en) | Method for controllably preparing FeNi3 micro-nano materials in various shapes | |
| CN111423622A (en) | Silicon dioxide nano composite reinforcing agent for hydrogenated nitrile rubber and preparation method thereof | |
| Wang et al. | CoS/Nitrogen-doped carbon composites derived from Zeolitic imidazolate frameworks-67 as advanced electrodes for supercapacitors | |
| CN111777063A (en) | Preparation method of nano material | |
| CN111748191A (en) | Two-dimensional graphene composite material with copper nanoparticles loaded on surface and preparation method and application thereof |
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 |
Application publication date: 20201016 |
|
| RJ01 | Rejection of invention patent application after publication |