CN112408494A - Preparation method of small-size ferric oxide cube - Google Patents
Preparation method of small-size ferric oxide cube Download PDFInfo
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- CN112408494A CN112408494A CN202011356495.3A CN202011356495A CN112408494A CN 112408494 A CN112408494 A CN 112408494A CN 202011356495 A CN202011356495 A CN 202011356495A CN 112408494 A CN112408494 A CN 112408494A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title description 3
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 title description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- SZQUEWJRBJDHSM-UHFFFAOYSA-N iron(3+);trinitrate;nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O SZQUEWJRBJDHSM-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 150000002505 iron Chemical class 0.000 claims description 4
- VXWSFRMTBJZULV-UHFFFAOYSA-H iron(3+) sulfate hydrate Chemical compound O.[Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VXWSFRMTBJZULV-UHFFFAOYSA-H 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims description 2
- VEPSWGHMGZQCIN-UHFFFAOYSA-H ferric oxalate Chemical compound [Fe+3].[Fe+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O VEPSWGHMGZQCIN-UHFFFAOYSA-H 0.000 claims description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 abstract 4
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 description 9
- 238000004729 solvothermal method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004626 scanning electron microscopy Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 238000004627 transmission electron microscopy Methods 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010626 work up procedure Methods 0.000 description 1
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- 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
- C01G49/06—Ferric oxide [Fe2O3]
-
- 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
- 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
-
- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Compounds Of Iron (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the technical field of controllable preparation of nanometer materials in shape and discloses small-size Fe2O3A preparation method of the cube. The preparation method takes N, N-Dimethylformamide (DMF) as a solvent and ferric salt as a precursor, and adopts a solvothermal route to successfully prepare Fe by a one-step method2O3Cubic, and the particle diameter is uniform and is 20-60 nm. The preparation process is simple, cheap in raw materials, good in repeatability, good in product crystallinity and suitable for large-scale industrial production.
Description
Technical Field
The invention belongs to the technical field of shape control of nano materials, relates to a nano material preparation technology based on a solvothermal method, and particularly relates to small-size ferric oxide Fe2O3A preparation method of the cube.
Background
The solvent thermal method refers to a closed system such as an autoclave, using organic or non-aqueous solvent as solventSolvent, at a certain temperature and the autogenous pressure of the solution, the original mixture is reacted. The method is simple, convenient and safe to operate, and is a technical means suitable for batch synthesis of the nano materials. However, due to the size effect of the nanomaterials, the surface energy is high during solvothermal processes, tending to form aggregates. Therefore, the prepared nano material has poor shape controllability and large granularity. In order to prepare small-sized nano-materials with controllable morphology, a proper surfactant is usually added to inhibit agglomeration of the nano-materials. The addition of surfactants increases the material production costs on the one hand and also increases the work-up burden on the other hand. In conclusion, the development of a preparation technology of a surfactant-free small-size nano material has important significance. In the invention, DMF is taken as a solvent, and a one-step solvothermal method is adopted to prepare small-size Fe2O3Cubic, which has important reference significance for the controllable preparation of small-size nano materials.
Disclosure of Invention
The invention aims to provide small-size Fe2O3The object of the invention is realized by the following technical steps:
small-size Fe2O3The preparation method of the cube comprises the following steps: dissolving a certain amount of iron salt in DMF, transferring to a hydrothermal kettle, reacting at 180 ℃ for 12h, centrifugally separating, drying and grinding to obtain small-size Fe2O3Cubic material.
In the above technical scheme, further, the volume of the materials in the hydrothermal kettle should be up to 80%.
Further, the adding amount of the iron salt and DMF is 1-10mmol:80 mL.
Further, the ferric salt is one of ferric chloride hexahydrate, ferric sulfate hydrate, ferric oxalate dihydrate and ferric nitrate nonahydrate. Preferably ferric nitrate nonahydrate.
Fe prepared by the invention2O3The cube particle size is 20-60 nm.
The invention has the beneficial effects that:
the invention adopts a one-step method to successfully prepare the small-size Fe with the size of about 50nm2O3The cube is simple in preparation process, good in repeatability, uniform in granularity of obtained products, good in crystallinity and beneficial to industrial scale production.
Drawings
FIG. 1 shows Fe prepared in example 12O3Scanning electron microscopy of (a).
FIG. 2 is Fe prepared in example 22O3Transmission electron microscopy images of (a).
FIG. 3 is Fe prepared in example 32O3X-ray diffraction pattern of (a).
Detailed Description
For better understanding of the present invention, the technical solutions of the present invention will be described below with reference to the accompanying drawings and the detailed description thereof
The present invention is not limited to the following examples.
Example 1
Small-size Fe2O3The preparation method of the cube comprises the following specific steps:
adding 1mmol ferric nitrate nonahydrate into 80mL DMF, transferring into 100mL hydrothermal kettle, reacting at 180 deg.C for 12h, centrifuging, drying, and grinding to obtain small-size Fe2O3Cubic material.
FIG. 1 shows small size Fe2O3Scanning electron microscopy of cubes. As can be seen from figure 1, the one-step method for preparing Fe by taking DMF as a solvent and ferric nitrate nonahydrate as a precursor is adopted by adopting a solvothermal route2O3Has obvious cubic characteristics, uniform size distribution and particle size of about 40-60 nm.
Example 2
Small-size Fe2O3The preparation method of the cube comprises the following specific steps:
2mmol of ferric nitrate nonahydrate was added to 80mL of DMF and then transferred to a 100mL hydrothermal kettle at 1Reacting for 12 hours at the temperature of 80 ℃, centrifugally separating, drying and grinding to obtain small-size Fe2O3Cubic material.
FIG. 2 is a small size Fe2O3Transmission electron microscopy of cubes. The Fe produced can be seen in the figure2O3Takes the shape of a cube with a size of about 50 nm.
Example 3
Small-size Fe2O3The preparation method of the cube comprises the following specific steps:
adding 5mmol of ferric sulfate hydrate into 80mL of DMF, transferring into a 100mL hydrothermal kettle, reacting at 180 ℃ for 12h, centrifuging, drying, and grinding to obtain small-size Fe2O3Cubic material.
FIG. 3 is a small size Fe2O3X-ray diffraction pattern of the cube. The Fe produced can be seen in the figure2O3The cube has good crystallinity and high purity, and corresponds to the standard card with the serial number of JCPDS No. 06-0502. It can be seen that the method of the invention can prepare Fe with small size, high purity and high crystallization quality in one step2O3Cubic and has excellent reproducibility.
Claims (5)
1. Small-size Fe2O3A method for preparing a cube, comprising: dissolving a certain amount of iron salt in DMF, transferring to a hydrothermal kettle, reacting at 180 ℃ for 12h, centrifugally separating, drying and grinding to obtain small-size Fe2O3Cubic material.
2. Small size Fe of claim 12O3The preparation method of the cube is characterized in that the volume of the materials in the hydrothermal kettle accounts for 80%.
3. Small size Fe of claim 12O3A method for preparing a cube, characterized in that the iron salt is reacted with DThe addition amount of MF was 1-10mmol:80 mL.
4. Small size Fe of claim 12O3The preparation method of the cube is characterized in that the ferric salt is one of ferric chloride hexahydrate, ferric sulfate hydrate, ferric oxalate dihydrate and ferric nitrate nonahydrate.
5. Small size Fe of claim 12O3Method for producing cubes, characterized in that Fe is produced2O3The cube particle size is 20-60 nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011356495.3A CN112408494B (en) | 2020-11-27 | 2020-11-27 | Preparation method of small-size ferric oxide cube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011356495.3A CN112408494B (en) | 2020-11-27 | 2020-11-27 | Preparation method of small-size ferric oxide cube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112408494A true CN112408494A (en) | 2021-02-26 |
| CN112408494B CN112408494B (en) | 2022-09-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011356495.3A Active CN112408494B (en) | 2020-11-27 | 2020-11-27 | Preparation method of small-size ferric oxide cube |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229900A (en) * | 2014-09-15 | 2014-12-24 | 济南大学 | Preparation method of alpha-Fe2O3 cubes |
| CN107265509A (en) * | 2017-06-19 | 2017-10-20 | 华南理工大学 | A kind of cubic nano-sized iron oxide and preparation method thereof |
| CN109306523A (en) * | 2018-09-02 | 2019-02-05 | 景德镇陶瓷大学 | It is a kind of to prepare monocrystalline Fe2O3The method of nano-particles self assemble square nanostructure |
-
2020
- 2020-11-27 CN CN202011356495.3A patent/CN112408494B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104229900A (en) * | 2014-09-15 | 2014-12-24 | 济南大学 | Preparation method of alpha-Fe2O3 cubes |
| CN107265509A (en) * | 2017-06-19 | 2017-10-20 | 华南理工大学 | A kind of cubic nano-sized iron oxide and preparation method thereof |
| CN109306523A (en) * | 2018-09-02 | 2019-02-05 | 景德镇陶瓷大学 | It is a kind of to prepare monocrystalline Fe2O3The method of nano-particles self assemble square nanostructure |
Non-Patent Citations (3)
| Title |
|---|
| 尹辉: "准立方体氧化铁纳米材料的制备及光催化性能研究", 《硅酸盐通报》 * |
| 杜庆波等: "溶剂热法制备A-Fe_2O_3纳米材料", 《光谱实验室》 * |
| 梁斌等: "一步溶剂热法制备石墨烯/Fe_2O_3复合材料及电容性能研究", 《化学研究与应用》 * |
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| CN112408494B (en) | 2022-09-06 |
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