CN107500363A - A kind of preparation method of prism hexa-prism nano-sized iron oxide - Google Patents
A kind of preparation method of prism hexa-prism nano-sized iron oxide Download PDFInfo
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- CN107500363A CN107500363A CN201710701084.5A CN201710701084A CN107500363A CN 107500363 A CN107500363 A CN 107500363A CN 201710701084 A CN201710701084 A CN 201710701084A CN 107500363 A CN107500363 A CN 107500363A
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 8
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 7
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims description 24
- 238000013019 agitation Methods 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000012360 testing method Methods 0.000 claims description 2
- 239000000047 product Substances 0.000 claims 4
- 239000006227 byproduct Substances 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 4
- 238000013461 design Methods 0.000 abstract description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 12
- 239000003054 catalyst Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002127 nanobelt Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
Classifications
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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]
-
- 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
-
- 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
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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
- C01P2004/10—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
-
- 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
-
- 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)
- Inorganic Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention belongs to technical field of nanometer material preparation, is related to a kind of preparation method of prism hexa-prism nano-sized iron oxide, and prism hexa-prism nanometer α Fe are prepared 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 specified temp, and single dispersing, the prism hexa-prism nanometer α Fe of high-purity is made2O3, its concrete technology step is prepared including solution 1, prepared by solution 2, prepared by mixed solution, sample preparation and finished product prepare five steps；Obtained finished product α Fe2O3In the shape of the prism of prism six, two bottom surfaces are regular hexagons, and its average-size is 550nm, average thickness 80nm；Its preparation technology 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, is had 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, is related to one kind and prepares the rib of prism six using hydro-thermal reaction method
Columnar nanometer iron oxide (α-Fe2O3) method, its product can be used as the fields such as electrode material, pigment, catalyst and magnetic recording material
Close.
Background technology：
Iron oxide (α-Fe2O3) it is a kind of typical low energy gap n-type semiconductor, its energy gap is 2.1eV.α-
Fe2O3Physics and chemical property with uniqueness, 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
With good weatherability, heat endurance it is good and the advantages of color gamut is wide, inorganic pigment and colouring agent can be used as；Nanometer α-Fe2O3
Also have the advantages that catalytic activity is high, selectivity is good and long lifespan, may be used as catalyst material.In addition, nanometer α-Fe2O3Also
With good magnetic, can be moved in externally-applied magnetic field along a direction, packing density is 10 times of general material, because
And it may be used as magnetic material and magnetic pipe recording material.In a word, nanometer α-Fe2O3In technologies such as light, electricity, medical science and bioengineering
Have a wide range of applications value and DEVELOPMENT PROSPECT in field.
At present, existing many methods can be used for preparing nanometer α-Fe2O3, such as flame thermal decomposition method, vapour deposition process, consolidate
Nanometer α-Fe prepared by Xiang Fa, masterplate method, chemical precipitation method, hydro-thermal method etc., wherein hydro-thermal method2O3With grain development is complete, group
The advantages that poly- mild degree, significantly improve the performance of material, it is considered to be one kind prepares a nanometer α-Fe2O3Important means.Grind
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-dimentional 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 to its performance, therefore prepares a kind of nanometer α-Fe of new pattern2O3There is weight to practical application
The meaning wanted.At present, on 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.
The content of the invention：
The shortcomings that it is an object of the invention to overcome prior art, seek design and a kind of method using hydro-thermal reaction is provided
Prepare prism hexa-prism nanometer α-Fe2O3New technology, its preparation technology is simple, and principle is reliable, and production cost is low, nothing
Pollution, material property are good.
In order to realize foregoing invention purpose, the inventive method is with FeCl3·6H2O and NaOH is raw material, second alcohol and water conduct
Solvent, 6-18 hours are reacted under the conditions of 180 DEG C, single dispersing, the prism hexa-prism nanometer α-Fe of high-purity is made2O3, its
Concrete technology step includes：
(1) prepared by solution 1：By 0.1302g FeCl3·6H2O is dissolved in 20mL absolute ethyl alcohol, and magnetic agitation is extremely
FeCl3·6H2O is completely dissolved, and obtains solution 1；
(2) prepared by solution 2：0.6g NaOH is dissolved in 40mL deionized water, magnetic agitation to NaOH is completely dissolved,
Obtain solution 2；
(3) prepared by mixed solution：The solution 2 obtained in step (2) is added dropwise in solution 1 with dropper, side edged
Magnetic agitation 10 minutes again after stirring and adding, obtain mixed solution；
(4) sample preparation：The mixed solution that step (3) obtains is transferred to the stainless steel cauldron of polytetrafluoroethyllining lining
In, reacted 18 hours under the conditions of 180 DEG C of temperature control, obtain solid violet brown Sample 38.5mg, its crystal structure is hexagonal crystal system；
(5) prepared by finished product：After the puce sample that step (4) is obtained uses deionized water and washes of absolute alcohol successively,
60 DEG C of drying of temperature control, obtain the nano-sized iron oxide (α-Fe of single dispersing prism hexa-prism2O3) finished product, its average-size is
550nm, average thickness 80nm, six sides are isosceles trapezoid, and two neighboring side surface direction is opposite.
Its preparation technology 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, and purity is high,
Had broad application prospects in terms of lithium ion battery negative material, be easy to carry out large-scale industrial production.
Brief description of the drawings：
Fig. 1 is prism hexa-prism nanometer α-Fe prepared by the present invention2O3XRD diffraction patterns, it is hexagonal crystal to show material
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) is prism
Hexa-prism α-Fe2O3Model, (b) are 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.
Embodiment：
The present invention is further elaborated below by specific embodiment and with reference to accompanying drawing.
Embodiment：
The present embodiment is related to a kind of specific processing step for preparing prism hexa-prism nano-sized iron oxide, its detailed process
Prepared including solution 1, prepared by solution 2, prepared by mixed solution, sample preparation and finished product prepare five steps：
(1) prepared by solution 1：By 0.1302g FeCl3·6H2O is dissolved in 20mL absolute ethyl alcohol, and magnetic agitation is extremely
FeCl3·6H2O is completely dissolved, and obtains solution 1；
(2) prepared by solution 2：0.6g NaOH is dissolved in 40mL deionized water, magnetic agitation to NaOH is completely dissolved,
Obtain solution 2；
(3) prepared by mixed solution：The solution 2 obtained in step (2) is added dropwise in solution 1 with dropper, side edged
Magnetic agitation 10 minutes again after stirring and adding, obtain mixed solution；
(4) sample preparation：The mixed solution that step (3) obtains is transferred to the stainless steel cauldron of polytetrafluoroethyllining lining
In, reacted 18 hours under the conditions of 180 DEG C of temperature control, obtain solid violet brown Sample 38.5mg, its crystal structure is hexagonal crystal system；
(5) prepared by finished product：After the puce sample that step (4) is obtained uses deionized water and washes of absolute alcohol successively,
60 DEG C of drying of temperature control, obtain the nano-sized iron oxide (α-Fe of single dispersing prism hexa-prism2O3) finished product, its 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 is in X-ray diffractometer (model：Rigaku SmartLab) and ESEM (model：
Hitachi S-4800) on detected；Wherein, Fig. 1 is the finished product XRD diffraction patterns of the present embodiment, specifically sweeping with 8 °/min
Speed is retouched to be scanned from 20 °~80 °；By comparing XRD standard cards, the diffraction pattern and α-Fe2O3Match, show oblique side
The product of face hexa-prism is α-Fe2O3；Fig. 2 (a) is the SEM top views of finished product, and as can be seen from the figure experiment is prepared
α-Fe2O3In the shape of the prism of prism six, two bottom surfaces are regular hexagons, and the average-size of finished product is 550nm, average thickness
Spend for 80nm；Fig. 2 (b) is the single α-Fe that the present embodiment obtains2O3SEM figure, it is in the rib of prism six that finished product, which can be clearly seen,
Rod structure, six sides are isosceles trapezoids, and adjacent two side surface directions are opposite；Size is 554nm, thickness 82nm；Fig. 3
(a) it is preferable prism hexa-prism α-Fe2O3Illustraton of model, by the bottom surface of two regular hexagons and the side of six isosceles trapezoids
Face forms, and two neighboring side surface direction is opposite；Fig. 3 (b) is made up of two { 0001 } bottom surfaces and six { 1123 } sides
Fe2O3The image that atom model is observed to obtain 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, its electrochemical property test result such as Fig. 4
It is shown.Under 100mA/g current density, after 100 circle charge and discharge cycles, the specific capacity of battery remains able to stable keep
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-sized iron oxide, it is characterised in that prepared using the method for hydro-thermal reaction
Prism hexa-prism nanometer α-Fe2O3, specific preparation process is prepared including solution 1, prepared by solution 2, prepared by mixed solution, sample
Prepared by product and finished product prepares five steps：
(1) prepared by solution 1：By 0.1302g FeCl3·6H2O is dissolved in 20mL absolute ethyl alcohol, magnetic agitation to FeCl3·
6H2O is completely dissolved, and obtains solution 1；
(2) prepared by solution 2：0.6g NaOH is dissolved in 40mL deionized water, magnetic agitation to NaOH is completely dissolved, and is obtained
Solution 2；
(3) prepared by mixed solution：The 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,
Reacted 18 hours under the conditions of 180 DEG C of temperature control, obtain solid violet brown Sample 38.5mg, its crystal structure is hexagonal crystal system；
(5) prepared by finished product：After the puce sample that step (4) is obtained uses deionized water and washes of absolute alcohol successively, temperature control
60 DEG C of drying, obtain the nano-sized iron oxide finished product of single dispersing prism hexa-prism, and its average-size is 550nm, average thickness
For 80nm, six sides are isosceles trapezoid, and two neighboring side surface direction is opposite.
A kind of 2. preparation method of prism hexa-prism nano-sized 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 its electrochemical property test result is 100mA/g's
Under current density, after 100 circle charge and discharge cycles, the specific capacity of battery remains able to be stably held in 418mAh/g, prepares
Prism hexa-prism α-Fe2O3There is cycle performance as lithium ion battery negative material.
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| CN108217751A (en) * | 2018-02-09 | 2018-06-29 | 青岛大学 | A kind of preparation method of hexa-prism alpha-FeOOH nano-rod |
| CN113201766A (en) * | 2021-05-06 | 2021-08-03 | 云南大学 | Preparation method of hematite photoanode |
| CN114956195A (en) * | 2022-06-21 | 2022-08-30 | 中国石油大学(北京) | Two-dimensional magnetic nano-particles and preparation method and application thereof |
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| 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 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217751A (en) * | 2018-02-09 | 2018-06-29 | 青岛大学 | A kind of preparation method of hexa-prism alpha-FeOOH nano-rod |
| CN113201766A (en) * | 2021-05-06 | 2021-08-03 | 云南大学 | Preparation method of hematite photoanode |
| CN113201766B (en) * | 2021-05-06 | 2022-03-29 | 云南大学 | Preparation method of hematite photoanode |
| CN114956195A (en) * | 2022-06-21 | 2022-08-30 | 中国石油大学(北京) | Two-dimensional magnetic nano-particles and preparation method and application thereof |
| 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 |
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