CN106946294A - Hollow structure Fe is carried out based on Hydrothermal Synthesiss2O3The method of preparation - Google Patents
Hollow structure Fe is carried out based on Hydrothermal Synthesiss2O3The method of preparation Download PDFInfo
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- CN106946294A CN106946294A CN201710231290.4A CN201710231290A CN106946294A CN 106946294 A CN106946294 A CN 106946294A CN 201710231290 A CN201710231290 A CN 201710231290A CN 106946294 A CN106946294 A CN 106946294A
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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
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- 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
- C01P2006/40—Electric properties
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- 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
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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
Abstract
The invention provides one kind hollow structure Fe is carried out based on Hydrothermal Synthesiss2O3The method of preparation, including weigh FeCl3·6H2O and urea, take ethylene glycol, pour into and fill FeCl3·6H2In the container of O and urea, magnet rotor is added, is fixed on magnetic stirring apparatus, stirring makes FeCl3·6H2O and urea are completely dissolved；Mixed solution is transferred in reactor, reacted in drying box；Reaction terminates rear question response kettle natural cooling, gained pelleting centrifugation is come out, with absolute ethyl alcohol and distilled water cyclic washing；By washed precipitation drying, the product for obtaining yellow green is FeOOH；Product is heated up, then natural cooling, obtain drying loose red product for Fe2O3.The present invention with higher capacity and extraordinary cycle performance, there is stronger magnetic, can there is good application prospect in terms of magnetic medicine carrier, microreactor as the negative material of lithium ion battery.
Description
Technical field
The present invention relates to one kind hollow structure Fe is carried out based on Hydrothermal Synthesiss2O3The method of preparation, belongs to hollow structure nanometer
Field of material preparation.
Background technology
Hollow structure nano material generates huge attraction in many existing and emerging sciemtifec and technical sphere.Due to
Hollow structure has bigger specific surface area and more surface atoms, therefore hollow nanometer material is shown and body material and reality
The different performance of heart particle nano material, such as special surface energy, optics, magnetics, catalysis performance, increasingly causes in recent years
The extensive concern of people.Hollow structure nano material is in terms of catalyst, drug release capsules, artificial cell, battery material
Application had important breakthrough.Using its internal space, nano hollow structure is used as storage and controlled release feature
Material, such as medicine, cosmetics, DNA.It is similar, the space inside hollow structure can be used to adjust the refractive index of catalyst,
Density and activity, number of times that increase catalyst may be reused etc..Before 1998, most hollow structure all limits to
In spherical, and it is micron-scale.Usually with spraying（spray-drying）Or air-blowing（gas-blowing）Method system
It is standby to obtain.Now, many synthetic methods are studied to be used, and size, shape, structure can be controlled, thus it is more more
Abundant hollow-core construction is successfully prepared out, and the research range of this is greatly open hollow nano-material is simultaneously
Excellent basis has been laid for its application.And the Fe of hollow-core construction2O3Nano material, due to its excellent performance, is always science
The emphasis of research, is widely used in terms of catalyst, pigment, gas sensitive, lithium ion battery.In view of its potential application
Value, the Fe of various structures2O3Nano material has been prepared out, such as nanotube, hollow ball, cup-like structure, hollow spindle
Shape structure, hollow core shell structure etc..
Preparation method in currently available technology is unable to prepare the Fe of corresponding hollow structure well2O3Material
Material, the efficiency of preparation is low, materials'use rate is not high.
The content of the invention
In view of in place of above-mentioned the deficiencies in the prior art, in being carried out it is an object of the invention to provide one kind based on Hydrothermal Synthesiss
Hollow structure Fe2O3The method of preparation.
The invention aims to overcome the shortcomings of material prepared by traditional preparation methods there is provided a kind of based on hydro-thermal
Synthesis carries out hollow structure Fe2O3The method of preparation.In order to achieve the above object, this invention takes following technical scheme：
The invention provides one kind hollow structure Fe is carried out based on Hydrothermal Synthesiss2O3The method of preparation, comprises the following steps：
Step 1: weighing FeCl3·6H2O and urea, take ethylene glycol, pour into and fill FeCl3·6H2In the container of O and urea,
Magnet rotor is added, is fixed on magnetic stirring apparatus, stirring makes FeCl3·6H2O and urea are completely dissolved；
Step 2: mixed solution is transferred in reactor, reacted 15 hours in drying box；
Step 3: reaction terminates rear question response kettle natural cooling, gained pelleting centrifugation is come out, it is anti-with absolute ethyl alcohol and distilled water
After backwashing is washed；
Step 4: by washed precipitation drying, the product for obtaining yellow green is FeOOH；
Step 5: product is warming up into 300 °C, then natural cooling, obtains drying loose red product for Fe2O3。
It is preferred that, FeCl in above-mentioned steps one3·6H2O is 0.135 g, and urea is 0.08 g, and ethylene glycol is 25ml.
It is preferred that, the reactor in above-mentioned steps two is 50ml, and the reactor for filling solution is anti-in 160 °C of drying box
Answer 15 hours.
It is preferred that, the reaction of above-mentioned steps three terminates rear question response kettle and naturally cools to room temperature, and gained pelleting centrifugation is come out,
With absolute ethyl alcohol and distilled water cyclic washing, the reagent complete to remove unreacted.
It is preferred that, washed being deposited under 60 °C is dried in vacuo 8h by above-mentioned steps four.
It is preferred that, above-mentioned steps five are warming up to 300 °C and are incubated 2 hours, then naturally cool to room temperature.
What the present invention was provided carries out hollow structure Fe based on Hydrothermal Synthesiss2O3The method of preparation, the hollow structure prepared
Fe2O3, have the hollow ball of magnetic loose structure, as the negative material of lithium ion battery, with higher capacity and very
Good cycle performance, has stronger magnetic, can there is good application prospect in terms of magnetic medicine carrier, microreactor.
Brief description of the drawings
The Fe that Fig. 1 is prepared for the present invention2O3Room temperature hysteresis curve schematic diagram；
Hollow structure α-the Fe that Fig. 2 is prepared for the present invention2O3It is 100mAg in current density−1Under first three circulation electricity
Pressure-capacity curve figure.
Embodiment
The present invention provides a kind of based on Hydrothermal Synthesiss progress hollow structure Fe2O3The method of preparation, to make the mesh of the present invention
, technical scheme and effect it is clearer, clear and definite, the present invention is described in more detail for the embodiment that develops simultaneously referring to the drawings.
It should be appreciated that specific embodiment described herein is not intended to limit the present invention only to explain the present invention.
What the present embodiment was provided carries out hollow structure Fe based on Hydrothermal Synthesiss2O3The method of preparation, specifically includes following step
Suddenly：
0.135 g FeCl respectively are weighed first3·6H2O and 0.08 g urea, add in beaker, 25ml second two are taken with graduated cylinder
Alcohol, pours into and fills FeCl3·6H2In the beaker of O and urea, magnet rotor will be added in beaker, be fixed on magnetic stirring apparatus,
Stirring makes FeCl under normal temperature3·6H2O and urea are completely dissolved.Mixed solution is transferred in 50ml reactor.Fill solution
Reactor reacted 15 hours in 160 °C of drying box.Reaction terminates rear question response kettle and naturally cools to room temperature, and gained is sunk
Shallow lake is centrifuged out, with absolute ethyl alcohol and distilled water cyclic washing, the reagent complete to remove unreacted.Washed is deposited in 60 °C
Lower vacuum drying 8h, the product for obtaining yellow green is FeOOH.Product is then placed in Muffle furnace, 300 °C of insulations 2 are warming up to small
When, room temperature is then naturally cooled to, it is Fe to finally obtain and dry loose red product2O3。
By experiment, it can be found that product is made up of microballoon.These microballoon sizes are than more uniform, and size is about in 3-5 μ
m.These microballoons are made up of nanometer sheet, can be obtained from damaged structure, these structures are hollow.Burnt by high temperature
Tie obtained Fe2O3.By the sample of high temperature sintering, pattern is not changed.This explanation sample has relatively good heat endurance.
The analysis of pattern and micro-structural is carried out to prepared sample with ESEM (SEM), structure is by nanometer sheet
The flower-like structure of composition, its size is about 5 μm.At this moment the pressure increase of reaction system, nanometer sheet is than larger and not hollow
Structure.When temperature reaches 200。C, more than the boiling point of ethylene glycol, the now viscosity reduction of reaction system, nanometer sheet difficulty is gathered into
Ball.It is appropriate to change FeCl3·6H2O and urea ratio, reaction temperature are constant, and the reaction time is shortened to 8h.What is obtained is still
The hollow nano-sphere of nanometer sheet composition, but compared to sample 1, Product size diminishes, and its size is about at 2-3 μm.
As shown in figure 1, being prepared Fe2O3 room temperature hysteresis curve figures.As illustrated, Fe2O3Show typical soft iron
Magnetic, its coercivity and remanent magnetization are 51.047 Oe and 20.985 emu/g respectively.This iron oxide is that have by nanometer
Piece composition, the loose structure of hollow structure is result in, the hollow ball of the loose structure of this magnetic can be carried magnetic and medicated
There is good application prospect in terms of body, microreactor.
As shown in Fig. 2 being Fe2O3It is 100 mAg in current density−1Under first three circulation voltage-specific capacity it is bent
Line chart, it can be seen that circulate in has discharge platform first near 0.85 V, discharge capacity is up to 1550.2 first
mAh·g−1, two discharge cycles after, capacity is respectively 479.9 mAhg−1With 293.8 mAhg−1, equivalent to head
The 40% of secondary discharge capacity and 19%.It can be seen that Fe2O3Electrode material capacity attenuation is than more serious, and irreversible loss is larger.
It is primarily due in assembling battery and capping processes, it is impossible to which control causes its invertibity poor under oxygen-free environment completely.
There are three aspect reasons in addition：One is that, because iron oxide material poorly conductive itself, intrinsic resistance is larger, is unfavorable for electronics and moves
Move.Two be the decomposition because electrolyte, forms one layer of organic film and is deposited on particle surface, that is, so-called SEI passivating films,
Three be probably caused by Lithium-ion embeding lattice a small amount of in circulating first.
What the present invention was provided carries out hollow structure Fe based on Hydrothermal Synthesiss2O3The method of preparation, the hollow structure prepared
Fe2O3, have the hollow ball of magnetic loose structure, as the negative material of lithium ion battery, with higher capacity and very
Good cycle performance, has stronger magnetic, can there is good application prospect in terms of magnetic medicine carrier, microreactor.
It is understood that for those of ordinary skills, can be with technique according to the invention scheme and its invention structure
Think of is subject to equivalent or change, and all these changes or replacement should all belong to the protection model of appended claims of the invention
Enclose.
Claims (2)
1. one kind carries out hollow structure Fe based on Hydrothermal Synthesiss2O3The method of preparation, it is characterised in that：The preparation method includes
Following steps：
Step 1: weighing FeCl3·6H2O and urea, take ethylene glycol, pour into and fill FeCl3·6H2In the container of O and urea, plus
Enter magnet rotor, be fixed on magnetic stirring apparatus, stirring makes FeCl3·6H2O and urea are completely dissolved；
Step 2: mixed solution is transferred in reactor, reacted in drying box；
Step 3: reaction terminates rear question response kettle natural cooling, gained pelleting centrifugation is come out, it is anti-with absolute ethyl alcohol and distilled water
After backwashing is washed；
Step 4: by washed precipitation drying, the product for obtaining yellow green is FeOOH；
Step 5: product is heated up, then natural cooling, obtains drying loose red product for Fe2O3。
2. carry out hollow structure Fe based on Hydrothermal Synthesiss as claimed in claim 12O3The method of preparation, it is characterised in that：It is described
Step 3 reaction terminates rear question response kettle and naturally cools to room temperature, gained pelleting centrifugation is come out, with absolute ethyl alcohol and distilled water
Cyclic washing, the reagent complete to remove unreacted.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710231290.4A CN106946294A (en) | 2017-04-11 | 2017-04-11 | Hollow structure Fe is carried out based on Hydrothermal Synthesiss2O3The method of preparation |
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| CN201710231290.4A CN106946294A (en) | 2017-04-11 | 2017-04-11 | Hollow structure Fe is carried out based on Hydrothermal Synthesiss2O3The method of preparation |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107706413A (en) * | 2017-11-08 | 2018-02-16 | 苏州宇量电池有限公司 | A kind of leaf Cyclic dart type iron oxide cathode material of nanometer three and preparation method thereof |
| CN108281636A (en) * | 2018-01-27 | 2018-07-13 | 景德镇陶瓷大学 | A kind of preparation method and applications of coated by titanium dioxide ferric oxide composite material |
| CN109411747A (en) * | 2018-10-18 | 2019-03-01 | 陕西科技大学 | A kind of urea acts on the preparation method of lower ultra-fine beta-FeOOH nanometer rods self assembly hollow out microballoon |
| CN114853082A (en) * | 2022-05-08 | 2022-08-05 | 西南石油大学 | Preparation method of spherical ferric oxide negative electrode material of lithium ion battery |
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| CN1986427A (en) * | 2005-12-21 | 2007-06-27 | 中国科学院化学研究所 | Nano ferric oxide material and its preparing process and use in water treatment |
| CN102659188A (en) * | 2012-05-22 | 2012-09-12 | 中北大学 | Magnetic ferric oxide micrometer flower material with multi-stage structure and preparation method thereof |
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2017
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| CN1986427A (en) * | 2005-12-21 | 2007-06-27 | 中国科学院化学研究所 | Nano ferric oxide material and its preparing process and use in water treatment |
| CN102659188A (en) * | 2012-05-22 | 2012-09-12 | 中北大学 | Magnetic ferric oxide micrometer flower material with multi-stage structure and preparation method thereof |
Non-Patent Citations (4)
| Title |
|---|
| LILI WANG, ET AL.: "Three-Dimensional Hierarchical Flowerlike α-Fe2O3 Nanostructures: Synthesis and Ethanol-Sensing Properties", 《APPLIED MATERIALS AND INTERFACES》 * |
| SHAO-WEN CAO, ET AL.: "Hierarchically Nanostructured Magnetic Hollow Spheres of Fe3O4 and γ-Fe2O3: Preparation and Potential Application in Drug Delivery", 《JOURNAL OF PHYSICAL CHEMISTRY C》 * |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107706413A (en) * | 2017-11-08 | 2018-02-16 | 苏州宇量电池有限公司 | A kind of leaf Cyclic dart type iron oxide cathode material of nanometer three and preparation method thereof |
| CN107706413B (en) * | 2017-11-08 | 2020-08-04 | 苏州宇量电池有限公司 | Nano three-leaf boomerang type iron oxide negative electrode material and preparation method thereof |
| CN108281636A (en) * | 2018-01-27 | 2018-07-13 | 景德镇陶瓷大学 | A kind of preparation method and applications of coated by titanium dioxide ferric oxide composite material |
| CN108281636B (en) * | 2018-01-27 | 2020-04-21 | 景德镇陶瓷大学 | Preparation method and application of titanium dioxide coated iron sesquioxide composite material |
| CN109411747A (en) * | 2018-10-18 | 2019-03-01 | 陕西科技大学 | A kind of urea acts on the preparation method of lower ultra-fine beta-FeOOH nanometer rods self assembly hollow out microballoon |
| CN109411747B (en) * | 2018-10-18 | 2021-03-16 | 陕西科技大学 | Preparation method of superfine beta-FeOOH nanorod self-assembled hollow microsphere under urea action |
| CN114853082A (en) * | 2022-05-08 | 2022-08-05 | 西南石油大学 | Preparation method of spherical ferric oxide negative electrode material of lithium ion battery |
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Application publication date: 20170714 |