CN107746081A - A kind of preparation method of two-dimensional nano piece form α Fe2O3 materials - Google Patents
A kind of preparation method of two-dimensional nano piece form α Fe2O3 materials Download PDFInfo
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- CN107746081A CN107746081A CN201711104420.4A CN201711104420A CN107746081A CN 107746081 A CN107746081 A CN 107746081A CN 201711104420 A CN201711104420 A CN 201711104420A CN 107746081 A CN107746081 A CN 107746081A
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- 239000000463 material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 title claims abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 32
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 14
- 239000011261 inert gas Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 238000010792 warming Methods 0.000 claims abstract description 7
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims description 18
- 229910000859 α-Fe Inorganic materials 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 230000001186 cumulative effect Effects 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- WOSISLOTWLGNKT-UHFFFAOYSA-L iron(2+);dichloride;hexahydrate Chemical compound O.O.O.O.O.O.Cl[Fe]Cl WOSISLOTWLGNKT-UHFFFAOYSA-L 0.000 claims 1
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 6
- DQMUQFUTDWISTM-UHFFFAOYSA-N O.[O-2].[Fe+2].[Fe+2].[O-2] Chemical compound O.[O-2].[Fe+2].[Fe+2].[O-2] DQMUQFUTDWISTM-UHFFFAOYSA-N 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 229960005191 ferric oxide Drugs 0.000 description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 9
- 239000002245 particle Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 239000011805 ball Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011806 microball Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- BYGOPQKDHGXNCD-UHFFFAOYSA-N tripotassium;iron(3+);hexacyanide Chemical compound [K+].[K+].[K+].[Fe+3].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-].N#[C-] BYGOPQKDHGXNCD-UHFFFAOYSA-N 0.000 description 2
- 206010013786 Dry skin Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 229940032296 ferric chloride Drugs 0.000 description 1
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- -1 potassium ferricyanide Chemical compound 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Classifications
-
- 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]
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/20—Two-dimensional structures
-
- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Iron (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a kind of two-dimensional nano piece form α Fe2O3The preparation method of material; the preparation method is that Iron(III) chloride hexahydrate is positioned in alumina crucible; it is then placed in the tube furnace equipped with alundum tube; inert gas is passed through after sealed; and 380 450 DEG C are warming up under protecting under an inert gas, kept for 8 24 hours, be subsequently cooled to room temperature; again after deionized water is washed, dried, two-dimensional nano piece form α Fe are obtained2O3Material.Compared with prior art, the present invention thermally decomposes oxidation reaction with Iron(III) chloride hexahydrate reagent under inert atmosphere protection and prepares two-dimensional nano piece form α Fe2O3Material, used reagent price is cheap, and preparation process is easier, prepare with scale can be achieved, and obtained di-iron trioxide pattern is two-dimensional nano piece.
Description
Technical field
The present invention relates to Two-dimensional morphology functional material to synthesize field, particularly a kind of two-dimensional nano piece form α-Fe2O3Material
Preparation method.
Background technology
α-Fe2O3Material is a kind of environmentally friendly type n semiconductor material, and less energy gap causes α-Fe2O3
Material has certain visible light-responded, its energy gap Eg=2.1 eV.Therefore, α-Fe2O3Material is widely applied to many
Field, such as lithium ion battery, gas sensor, photocatalysis, water process and photocatalysis Decomposition aquatic products hydrogen etc..Also, α-Fe2O3
Material also has the advantage such as nontoxic, cheap and easy to get, so, α-Fe2O3Material is studied by increasing people in recent years, mesh
Before, nanometer alpha-Fe2O3The preparation method of material has following several：Hydrolyze method, hydro-thermal method, sol-gel process, spray-wall interaction
Method, microemulsion method, the precipitation method, masterplate method, electrochemistry anodic oxidation and magnetron sputtering method etc..
China Patent Publication No. CN101475223A discloses a kind of nanostructured alpha type ferric oxide hollow submicrosphere
Preparation method.This method is by by after ferrous salt and the reaction of complexant hydrofluoric acid, adding ammoniacal liquor regulation pH value, then adding template
(nearly monodispersed SiO2Or PS sub-micros ball) reaction obtain nanostructured nucleocapsid sub-micro ball, finally remove removing template, obtain nano junction
The hollow sub-micro ball of structure alpha-type ferric oxide.
China Patent Publication No. CN101693600A discloses a kind of preparation method of ferric oxide film.This method is first
Ferric chloride hexahydrate crystal is first dissolved in ethylene glycol solvent and is made into ferric chloride solution, ethylenediamine liquid is dissolved in into ethanol is made into second two
Amine aqueous solution, it is 5.5~6.5 that then ethylenediamine solution, which is added in cobalt chloride solution to pH value, forms mixed solution；Will mixing
Solution is incubated 6~20 hours under the conditions of 20~60 DEG C and forms colloidal sol；Colloidal sol is coated on glass using czochralski method, 30~
60 DEG C of dryings 0.5~5 hour, form gel mould；Gel mould on glass is heated, 30 are heat-treated under the conditions of 400~500 DEG C
~60 minutes, form ferric oxide film.
China Patent Publication No. CN101698515A discloses a kind of preparation method of alpha-phase ferricoxide nanospheres.The preparation
Method, by hydro-thermal method in certain temperature and time, can be divided first using inorganic molysite and acid phosphate as raw material
Dissipate good property, narrow particle size distribution, the alpha-phase ferricoxide nano particle with spherical structure.
China Patent Publication No. CN101928043A discloses a kind of alpha-type ferric oxide micron ball and preparation method thereof.
This method prepares water-soluble iron potassium cyanide solution and sodium hydroxide solution respectively, by water-soluble iron potassium cyanide solution and sodium hydroxide
Solution mixes, and obtains mixed liquor；Trisodium citrate is added in mixed liquor, it is fully dissolved after ultrasound, it is molten to obtain faint yellow clarification
Liquid；The faint yellow settled solution of gained is transferred in stainless steel cauldron, temperature reaction；Product cooling after temperature reaction
To room temperature, washed after bottom sediment is centrifuged, products therefrom is dried, produces alpha-type ferric oxide micron ball.
China Patent Publication No. CN102826612A discloses a kind of preparation side of three-dimensional flower-shaped structure alpha-type ferric oxide
Method.This method prepares potassium ferricyanide solution respectively first and sodium hydroxide solution remixes, and obtains mixed liquor；Secondly added in liquid
Urea, obtain faint yellow settled solution；Finally the faint yellow settled solution of gained is transferred in reactor, seals and heats up anti-
Should, after product is cooled to room temperature, wash, dry after bottom sediment is centrifuged, produce the three-dimensional flower-shaped oxidation of α types three two
Iron.
These above-mentioned di-iron trioxide material preparation methods, more using raw material type, preparation process is complicated, is used
Reagent and equipment price it is higher, and resulting product is thin for three-dimensional spherical, flower-shaped di-iron trioxide or di-iron trioxide
Film.
The content of the invention
The invention aims to solve the problems, such as that prior art preparation process is complicated and production cost is high, this hair
Bright provide a kind of thermally decomposes oxidation reaction system using cheap Iron(III) chloride hexahydrate reagent under inert atmosphere protection
Standby two-dimensional nano piece form α-Fe2O3The method of material.
A kind of two-dimensional nano piece form α-Fe2O3The preparation method of material, comprises the following steps：
Step 1: taking Iron(III) chloride hexahydrate to be positioned in alumina crucible, the Iron(III) chloride hexahydrate loadings are with volume
Measure as 0.1-0.5 times of alumina crucible cumulative volume, then alumina crucible is put into the tube furnace equipped with alundum tube, two
End sealing；
Step 2: being passed through inert gas into tube furnace, and 380-450 DEG C is warming up under protecting under an inert gas, keeps 8-
24 hours, it is subsequently cooled to room temperature；
Step 3: after the product taken out in alumina crucible is washed through deionized water, dried, obtain two-dimensional nano piece form α-
Fe2O3Material.
Further, the alumina crucible equipped with Iron(III) chloride hexahydrate is with cover, and be positioned over the tube furnace of alundum tube
Center.
Preferably, the inert gas in the step 2 is more than one or both of nitrogen, helium, argon gas gas
Flow is in 100-200 mL/min.
Preferably, heating rate is 5-10 DEG C/min in the step 2.
Compared with prior art, the present invention thermally decomposes oxidation instead with Iron(III) chloride hexahydrate reagent under inert atmosphere protection
Two-dimensional nano piece form α-Fe should be prepared2O3Material, used reagent price is cheap, and preparation process is easier, and scale can be achieved
Change and prepare, and obtained di-iron trioxide pattern is two-dimensional nano piece.
Brief description of the drawings
Fig. 1 is two-dimensional nano piece form α-Fe prepared by the embodiment of the present invention 12O3The SEM photograph of material.
Fig. 2 is two-dimensional nano piece form α-Fe prepared by the embodiment of the present invention 22O3The SEM photograph of material.
Fig. 3 is two-dimensional nano piece form α-Fe prepared by the embodiment of the present invention 32O3The SEM photograph of material.
Fig. 4 is two-dimensional nano piece form α-Fe prepared by the embodiment of the present invention 42O3The SEM photograph of material.
Fig. 5 is two-dimensional nano piece form α-Fe prepared by the embodiment of the present invention 12O3The XRD spectra of material.
Embodiment
With reference to specific embodiment, the invention will be further described, the illustrative examples and explanation invented herein
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1
25 mL Iron(III) chloride hexahydrate solid particles will be loaded in 50 mL alumina crucible, after alumina crucible capping, put
Enter in the tube furnace equipped with alundum tube, after tube furnace both ends are sealed, be passed through nitrogen with 100 mL/min flows and purge 10 minutes,
Then 380 DEG C are warming up to 5 DEG C/min speed, and are kept for 24 hours, be subsequently cooled to room temperature, taken out in alumina crucible
Product obtains two-dimensional nano piece form α-Fe after deionized water is washed, dried2O3Material, by two wieners made from embodiment 1
Rice piece form α-Fe2O3Material characterizes to obtain SEM photograph under a scanning electron microscope, as shown in figure 1, as can be seen from Figure 1
α-Fe made from the present embodiment2O3Material, its pattern are two-dimensional nano piece, the nm of thickness about 100 ~ 500, and accumulate it is closer, then
By to two-dimensional nano piece form α-Fe made from embodiment 12O3Material carries out X-ray diffraction, analyzes its diffracting spectrum, such as Fig. 5
It is shown, obtain diffraction maximum and correspond respectively to α-Fe2O3(012), (104), (110), (113), (024), (116),
(018), (214) and (300) crystal face.
Embodiment 2
20 mL Iron(III) chloride hexahydrate solid particles will be loaded in 50 mL alumina crucible, after alumina crucible capping, put
Enter in the tube furnace equipped with alundum tube, after tube furnace both ends are sealed, be passed through nitrogen with 100 mL/min flows and purge 10 minutes,
Then 400 DEG C are warming up to 10 DEG C/min speed, and are kept for 20 hours, be subsequently cooled to room temperature, taken out in alumina crucible
Product wash through deionized water, dry after, obtain two-dimensional nano piece form α-Fe2O3Material, will be two-dimentional made from embodiment 2
Nanometer sheet form α-Fe2O3Material characterizes to obtain SEM photograph under a scanning electron microscope, as shown in Fig. 2 can from Fig. 2
Go out α-Fe made from the present embodiment2O3Material, its pattern are two-dimensional nano piece, the nm of thickness about 200 ~ 400, and are accumulated closer.
Embodiment 3
10 mL Iron(III) chloride hexahydrate solid particles will be loaded in 50 mL alumina crucible, after alumina crucible capping, put
Enter in the tube furnace equipped with alundum tube, after tube furnace both ends are sealed, be passed through nitrogen with 200 mL/min flows and purge 10 minutes,
Then 420 DEG C are warming up to 10 DEG C/min speed, and are kept for 12 hours, be subsequently cooled to room temperature, taken out in alumina crucible
Product wash through deionized water, dry after, obtain two-dimensional nano piece form α-Fe2O3Material, will be two-dimentional made from embodiment 3
Nanometer sheet form α-Fe2O3Material characterizes to obtain SEM photograph under a scanning electron microscope, as shown in figure 3, can from Fig. 3
Go out α-Fe made from the present embodiment2O3Material, its pattern are two-dimensional nano piece, the nm of thickness about 80 ~ 100, and are accumulated loosely.
Embodiment 4
5 mL Iron(III) chloride hexahydrate solid particles will be loaded in 50 mL alumina crucible, after alumina crucible capping, be put into
In tube furnace equipped with alundum tube, after tube furnace both ends are sealed, nitrogen purging is passed through 10 minutes with 200 mL/min flows, so
450 DEG C are warming up to 10 DEG C/min speed afterwards, and is kept for 8 hours, is subsequently cooled to room temperature, takes out the production in alumina crucible
Thing obtains two-dimensional nano piece form α-Fe after deionized water is washed, dried2O3Material, by two-dimensional nano made from embodiment 4
Piece form α-Fe2O3Material characterizes to obtain SEM photograph under a scanning electron microscope, as shown in figure 4, as can be seen from Figure 4 originally
α-Fe made from embodiment2O3Material, its pattern are two-dimensional nano piece, the nm of thickness about 100 ~ 800, and are accumulated loosely.
Technical scheme is not limited to the limitation of above-mentioned specific embodiment, and every technique according to the invention scheme is done
The technology deformation gone out, each falls within protection scope of the present invention.
Claims (4)
- A kind of 1. two-dimensional nano piece form α-Fe2O3The preparation method of material, it is characterised in that comprise the following steps：Step 1: taking Iron(III) chloride hexahydrate to be positioned in alumina crucible, the Iron(III) chloride hexahydrate loadings are with volume Measure as 0.1-0.5 times of alumina crucible cumulative volume, then alumina crucible is put into the tube furnace equipped with alundum tube, two End sealing；Step 2: being passed through inert gas into tube furnace, and 380-450 DEG C is warming up under protecting under an inert gas, keeps 8- 24 hours, it is subsequently cooled to room temperature；Step 3: after the product taken out in alumina crucible is washed through deionized water, dried, obtain two-dimensional nano piece form α- Fe2O3Material.
- 2. two-dimensional nano piece form α-Fe according to claim 12O3The preparation method of material, it is characterised in that：Equipped with six The alumina crucible of iron chloride hexahydrate is with cover, and is positioned over the center of the tube furnace of alundum tube.
- 3. two-dimensional nano piece form α-Fe according to claim 12O3The preparation method of material, it is characterised in that：The step Inert gas in rapid two is that more than one or both of nitrogen, helium, argon gas gas flow is in 100-200 mL/min.
- 4. two-dimensional nano piece form α-Fe according to claim 12O3The preparation method of material, it is characterised in that：The step Heating rate is 5-10 DEG C/min in rapid two.
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| CN117446871A (en) * | 2023-10-13 | 2024-01-26 | 湖北江城实验室 | Two-dimensional ferric oxide nano-sheet and preparation method thereof |
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| CN105776348A (en) * | 2016-05-03 | 2016-07-20 | 陕西理工学院 | Simple preparation method for micron-order magnetic alpha-iron trioxide particles |
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| CN105776348A (en) * | 2016-05-03 | 2016-07-20 | 陕西理工学院 | Simple preparation method for micron-order magnetic alpha-iron trioxide particles |
Non-Patent Citations (1)
| Title |
|---|
| JUN WANG ET AL.: "Crystal shape and orientation controlled α-Fe2O3 nanoparticles prepared by decarbonation of FeCO3", 《MODERN PHYSICS LETTERS B》 * |
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| CN117446871A (en) * | 2023-10-13 | 2024-01-26 | 湖北江城实验室 | Two-dimensional ferric oxide nano-sheet and preparation method thereof |
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