CN107500363B - A kind of preparation method of prism hexa-prism nano iron oxide - Google Patents
A kind of preparation method of prism hexa-prism nano iron oxide Download PDFInfo
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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)
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/11—Particle morphology extending in one dimension, e.g. needle-like with a prismatic shape
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention belongs to technical field of nanometer material preparation, are related to a kind of preparation method of prism hexa-prism nano iron oxide, prepare prism hexa-prism nanometer α-Fe using the method for hydro-thermal reaction2O3New material；With FeCl3·6H2O and NaOH is raw material, and second alcohol and water is solvent, is reacted under conditions of specific temperature, and the prism hexa-prism nanometer α-Fe of monodisperse, high-purity is made2O3, specific process step includes that the preparation of solution 1, the preparation of solution 2, mixed solution preparation, sample preparation and finished product prepare five steps；Obtained finished product α-Fe2O3In the shape of prism hexagonal prisms, two bottom surfaces are regular hexagon, average-size 550nm, average thickness 80nm；Its preparation process is simple, and operation is nimble, and design principle is reliable, and production cost is low, and product yield is high, and application environment is friendly, the α-Fe prepared2O3Monodispersity is good, and purity is high has broad application prospects in terms of lithium ion battery negative material, is easy to carry out large-scale industrial production.
Description
Technical field:
The invention belongs to technical field of nanometer material preparation, it is related to a kind of preparing six rib of prism using hydro-thermal reaction method
Columnar nanometer iron oxide (α-Fe2O3) method, product can be used as the fields such as electrode material, pigment, catalyst and magnetic recording material
It closes.
Background technique:
Iron oxide (α-Fe2O3) it is a kind of typical low energy gap n-type semiconductor, forbidden bandwidth 2.1eV.α-
Fe2O3With unique physics and chemical property, make it that there is wide answer in the technical fields such as light, electricity, magnetic and bioengineering
With prospect, the extensive concern of people is caused.Nanometer α-Fe2O3With theoretical specific capacity height (1007mAh g-1), rich reserves,
Stability is good, non-toxic and cheap the advantages that easily obtaining, and may be used as lithium ion battery negative material；Meanwhile nanometer α-Fe2O3
Have the advantages that good weatherability, thermal stability are good and color gamut is wide, can be used as inorganic pigment and colorant；Nanometer α-Fe2O3
Also have many advantages, such as that catalytic activity is high, selectivity is good and the service life is long, may be used as catalyst material.In addition, nanometer α-Fe2O3Also
With good magnetism, can be moved along a direction in externally-applied magnetic field, packing density is 10 times of general substance, because
And it may be used as magnetic material and magnetic pipe recording material.In short, nanometer α-Fe2O3In technologies such as light, electricity, medicine and bioengineering
The value that has a wide range of applications in field and development prospect.
Currently, having many methods can be used for preparing a nanometer α-Fe2O3, such as flame thermal decomposition method, vapour deposition process, consolidate
Xiang Fa, template method, chemical precipitation method, hydro-thermal method etc., the nanometer α-Fe that wherein prepared by hydro-thermal method2O3, group complete with grain development
The advantages that poly- mild degree, significantly improves the performance of material, it is considered to be a kind of to prepare a nanometer α-Fe2O3Important means.It grinds
The person of studying carefully utilizes these synthetic methods, prepares the nanometer α-Fe of a variety of different-shapes2O3, such as the nano particle of zero dimension
(W.T.Zhang, J.Mater.Chem., 2002,12:1676) etc., one-dimensional nano wire (Y.L.Chueh, M.W.Lai,
J.Q.Liang, L.J.Chou, Z.L.Wang, Adv.Funct.Mater., 2006,16:2243), nanotube (J.Chen,
L.Xu, W.Li, X.Gou, Adv.Mater., 2005,17:582), nanobelt (Z.W.Pan, Z.R.Dai, Z.L.Wang,
Science, 2001,291:1947) etc., two-dimensional nanometer sheet (L.Liao, Z.Zheng, B.Yan, J.X.Zhang, H.Gong,
J.C.Li, C.Liu, Z.X.Shen, T.Yu, J.Phys.Chem.C, 2008,112:10784) etc., three-dimensional nanocube
(P.R.Patil, S.S.Joshi, Synth.React.Inorg.M., 2007,37:425), hexa-prism (D.F.Peng,
S.Beysen, Q.Li, Y.F.Sun, L.Y.Yang, Particuology, 2010,8:386) etc..Due to α-Fe2O3Pattern and
Structure has a very big impact its performance, therefore prepares a kind of nanometer α-Fe of novel pattern2O3There is weight to practical application
The meaning wanted.Currently, about prism hexa-prism nanometer α-Fe2O3Preparation and its application there is not been reported, especially with
Hydro-thermal reaction method prepares prism hexa-prism nanometer α-Fe2O3Technological means there is not been reported.
Summary of the invention:
The purpose of the present invention is to overcome the shortcomings of the existing technology, seeks design and provides a kind of method using hydro-thermal reaction
Prepare prism hexa-prism nanometer α-Fe2O3New process, preparation process is simple, and principle is reliable, and production cost is low, nothing
Pollution, material property are good.
In order to achieve the above-mentioned object of the invention, the method for the present invention is with FeCl3·6H2O and NaOH is raw material, second alcohol and water conduct
Solvent reacts 6-18 hours under the conditions of 180 DEG C, and the prism hexa-prism nanometer α-Fe of monodisperse, high-purity is made2O3,
Specific process step includes:
(1) prepared by solution 1: by the FeCl of 0.1302g3·6H2O is dissolved in the dehydrated alcohol of 20mL, and magnetic agitation is extremely
FeCl3·6H2O is completely dissolved, and obtains solution 1；
(2) prepared by solution 2: the NaOH of 0.6g is dissolved in the deionized water of 40mL, magnetic agitation to NaOH is completely dissolved,
Obtain solution 2；
(3) prepared by mixed solution: solution 2 obtained in step (2) being added dropwise in solution 1 with dropper, side edged
Magnetic agitation 10 minutes again after stirring and adding, obtain mixed solution；
(4) mixed solution that step (3) obtains sample preparation: is transferred to the stainless steel cauldron of polytetrafluoroethyllining lining
In, it is reacted 18 hours under the conditions of 180 DEG C of temperature control, obtains solid violet brown Sample 38.5mg, crystal structure is hexagonal crystal system；
(5) prepared by finished product: after the puce sample that step (4) obtains successively is used deionized water and washes of absolute alcohol,
60 DEG C of temperature control drying, obtain the nano iron oxide (α-Fe of monodisperse prism hexa-prism2O3) finished product, average-size is
550nm, average thickness 80nm, six sides are isosceles trapezoid, and two neighboring side surface direction is opposite.
Its preparation process is simple compared with prior art by the present invention, and operation is nimble, and design principle is reliable, and production cost is low,
Product yield is high, and application environment is friendly, the prism hexa-prism nanometer α-Fe prepared2O3Monodispersity is good, purity is high,
It is had broad application prospects in terms of lithium ion battery negative material, is easy to carry out large-scale industrial production.
Detailed description of the invention:
Fig. 1 is prism hexa-prism nanometer α-Fe prepared by the present invention2O3XRD diffraction pattern, show material be hexagonal crystal
Monocrystalline α-the Fe of phase structure2O3。
Fig. 2 is prism hexa-prism nanometer α-Fe prepared by the present invention2O3SEM image, wherein (a) be SEM overlook
Figure (b) is single prism hexa-prism nanometer α-Fe2O3SEM image.
Fig. 3 is prism hexa-prism nanometer α-Fe prepared by the present invention2O3Model schematic, wherein (a) be prism
Hexa-prism α-Fe2O3Model (b) is prism hexa-prism α-Fe2O3Atom model [0001] direction projection figure.
Fig. 4 is prism hexa-prism nanometer α-Fe prepared by the present invention2O3Chemical property figure.
Specific embodiment:
The present invention is further elaborated below by specific embodiment and in conjunction with attached drawing.
Embodiment:
The present embodiment is related to a kind of processing step for specifically preparing prism hexa-prism nano iron oxide, detailed process
Five steps are prepared including the preparation of solution 1, the preparation of solution 2, mixed solution preparation, sample preparation and finished product:
(1) prepared by solution 1: by the FeCl of 0.1302g3·6H2O is dissolved in the dehydrated alcohol of 20mL, and magnetic agitation is extremely
FeCl3·6H2O is completely dissolved, and obtains solution 1；
(2) prepared by solution 2: the NaOH of 0.6g is dissolved in the deionized water of 40mL, magnetic agitation to NaOH is completely dissolved,
Obtain solution 2；
(3) prepared by mixed solution: solution 2 obtained in step (2) being added dropwise in solution 1 with dropper, side edged
Magnetic agitation 10 minutes again after stirring and adding, obtain mixed solution；
(4) mixed solution that step (3) obtains sample preparation: is transferred to the stainless steel cauldron of polytetrafluoroethyllining lining
In, it is reacted 18 hours under the conditions of 180 DEG C of temperature control, obtains solid violet brown Sample 38.5mg, crystal structure is hexagonal crystal system；
(5) prepared by finished product: after the puce sample that step (4) obtains successively is used deionized water and washes of absolute alcohol,
60 DEG C of temperature control drying, obtain the nano iron oxide (α-Fe of monodisperse prism hexa-prism2O3) finished product, average-size is
550nm, average thickness 80nm, six sides are isosceles trapezoid, and two neighboring side surface direction is opposite.
The finished product that the present embodiment obtains X-ray diffractometer (model: Rigaku SmartLab) and scanning electron microscope (model:
Hitachi S-4800) on detected；Wherein, Fig. 1 is the finished product XRD diffraction pattern of the present embodiment, specifically sweeping with 8 °/min
Rate is retouched to be scanned from 20 °~80 °；By comparing XRD standard card, the diffraction pattern and α-Fe2O3Match, shows oblique side
The product of face hexa-prism is α-Fe2O3；Fig. 2 (a) is the SEM top view of finished product, and as can be seen from the figure experiment is prepared
α-Fe2O3In the shape of prism hexagonal prisms, two bottom surfaces are regular hexagons, and the average-size of finished product is 550nm, average thickness
Degree is 80nm；Fig. 2 (b) is the single α-Fe that the present embodiment obtains2O3SEM figure, finished product can be clearly seen in six rib of prism
Rod structure, six sides are isosceles trapezoids, and two adjacent side surface directions are opposite；Having a size of 554nm, with a thickness of 82nm；Fig. 3
It (a) is ideal prism hexa-prism α-Fe2O3Illustraton of model, by the bottom surface of two regular hexagons and the side of six isosceles trapezoids
Face composition, and two neighboring side surface direction is opposite；Fig. 3 (b) is made of two { 0001 } bottom surfaces and six { 1123 } sides
Fe2O3The image that atom model is observed along [0001] direction, the prism hexa-prism nanometer being prepared with the present embodiment
α-Fe2O3Angle and profile coincide.
The finished product of the present embodiment is applied in lithium ion battery negative material occasion, electrochemical property test result such as Fig. 4
It is shown.Under the current density of 100mA/g, after 100 circle charge and discharge cycles, the specific capacity of battery still is able to stablize holding
In 418mAh/g, show prepared prism hexa-prism α-Fe2O3There is good follow as lithium ion battery negative material
Ring performance.
Claims (2)
1. a kind of preparation method of prism hexa-prism nano iron oxide, it is characterised in that prepared using the method for hydro-thermal reaction
Prism hexa-prism nanometer α-Fe2O3, specific preparation process includes the preparation of solution 1, the preparation of solution 2, mixed solution preparation, sample
Product preparation and finished product prepare five steps:
(1) prepared by solution 1: by the FeCl of 0.1302g3·6H2O is dissolved in the dehydrated alcohol of 20mL, magnetic agitation to FeCl3·
6H2O is completely dissolved, and obtains solution 1；
(2) prepared by solution 2: the NaOH of 0.6g being dissolved in the deionized water of 40mL, magnetic agitation to NaOH is completely dissolved, and is obtained
Solution 2；
(3) prepared by mixed solution: solution 2 obtained in step (2) is added dropwise in solution 1 with dropper, it is stirring while adding
And magnetic agitation 10 minutes again after adding, obtain mixed solution；
(4) sample preparation: the mixed solution that step (3) obtains is transferred in the stainless steel cauldron of polytetrafluoroethyllining lining,
It is reacted 18 hours under the conditions of 180 DEG C of temperature control, obtains solid violet brown Sample 38.5mg, crystal structure is hexagonal crystal system；
(5) prepared by finished product: after the puce sample that step (4) obtains successively is used deionized water and washes of absolute alcohol, temperature control
60 DEG C of drying, obtain the nano iron oxide finished product of monodisperse prism hexa-prism, average-size 550nm, average thickness
For 80nm, six sides are isosceles trapezoid, and two neighboring side surface direction is opposite.
2. a kind of preparation method of prism hexa-prism nano iron oxide according to claim 1, it is characterised in that system
Standby iron oxide finished product is applied in lithium ion battery negative material occasion, and electrochemical property test result is 100mA/g's
Under current density, after 100 circle charge and discharge cycles, the specific capacity of battery still is able to be stably held in 418mAh/g, preparation
Prism hexa-prism α-Fe2O3There is cycle performance as lithium ion battery negative material.
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| CN108217751B (en) * | 2018-02-09 | 2020-04-24 | 青岛大学 | Preparation method of hexagonal prism α -FeOOH nanorod |
| CN113201766B (en) * | 2021-05-06 | 2022-03-29 | 云南大学 | Preparation method of hematite photoanode |
| CN114956195B (en) * | 2022-06-21 | 2023-11-03 | 中国石油大学(北京) | Two-dimensional magnetic nanoparticle and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974413A (en) * | 2006-11-21 | 2007-06-06 | 浙江大学 | Process of preparing nanometer hexagonal oxide sheet |
| CN101088919A (en) * | 2006-06-13 | 2007-12-19 | 中国科学院福建物质结构研究所 | Nanometer iron oxide yellow as water purifying material and its synthesis process and use |
| CN101293675A (en) * | 2008-06-12 | 2008-10-29 | 浙江大学 | Method for preparing hexagonal disc shaped alpha-Fe2O3 powder |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101088919A (en) * | 2006-06-13 | 2007-12-19 | 中国科学院福建物质结构研究所 | Nanometer iron oxide yellow as water purifying material and its synthesis process and use |
| CN1974413A (en) * | 2006-11-21 | 2007-06-06 | 浙江大学 | Process of preparing nanometer hexagonal oxide sheet |
| CN101293675A (en) * | 2008-06-12 | 2008-10-29 | 浙江大学 | Method for preparing hexagonal disc shaped alpha-Fe2O3 powder |
Non-Patent Citations (3)
| Title |
|---|
| Hydrothermal synthesis of monodisperse α-Fe2O3 hexagonal platelets;Dengfeng Peng, et al.;《Particuology》;20101231;第8卷;386-389 * |
| Low-temperature synthesis ofα-Fe2O3hexagonal nanoparticles for environmental remediation and smart sensor applications;Ahmad Umar, et al.;《Talanta》;20130823;第116卷;1060-1066 * |
| Successful Hydrothermal Synthesis of α-Fe2O3Hexagonal Micro-platelets and Its Application in Li-Ion Battery;Huang Lihong, et al.;《Rare Metal Materials and Engineering》;20131031;第42卷(第10期);2014-2018 * |
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