CN107746081B - A kind of two-dimensional nano piece form α-Fe2O3The preparation method of material - Google Patents
A kind of two-dimensional nano piece form α-Fe2O3The preparation method of material Download PDFInfo
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- CN107746081B CN107746081B CN201711104420.4A CN201711104420A CN107746081B CN 107746081 B CN107746081 B CN 107746081B CN 201711104420 A CN201711104420 A CN 201711104420A CN 107746081 B CN107746081 B CN 107746081B
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- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 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 36
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims abstract description 18
- 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
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000007789 sealing Methods 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
- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 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
- 229910000859 α-Fe Inorganic materials 0.000 abstract description 16
- 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
- 238000005406 washing Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 description 16
- 239000000243 solution Substances 0.000 description 14
- 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
- 229910052571 earthenware Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000011806 microball 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
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000011805 ball Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000010408 film Substances 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
- 238000002156 mixing Methods 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
- 238000000926 separation method Methods 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
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 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
- 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
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 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
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 230000002349 favourable effect 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
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000002086 nanomaterial Substances 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
- 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
- 239000010409 thin film Substances 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 placed in alumina crucible; it is then placed in the tube furnace equipped with alundum tube; inert gas is passed through after sealed; and it is warming up to 380-450 DEG C under protecting under an inert gas, it is kept for 8-24 hours, is then cooled to room temperature; again after deionized water washing, dry, two-dimensional nano piece form α-Fe is obtained2O3Material.Compared with prior art, the present invention thermally decomposes oxidation reaction preparation two-dimensional nano piece form α-Fe with Iron(III) chloride hexahydrate reagent under inert atmosphere protection2O3Material, used reagent price is cheap, and preparation process is easier, it can be achieved that prepare with scale, and obtained di-iron trioxide pattern is two-dimensional nano piece.
Description
Technical field
The present invention relates to Two-dimensional morphology functional materials to synthesize field, especially a kind of two-dimensional nano piece form α-Fe2O3Material
Preparation method.
Background technique
α-Fe2O3Material is a kind of environmentally friendly type n semiconductor material, and lesser forbidden bandwidth makes α-Fe2O3
Material has certain visible light-responded, forbidden bandwidth 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 advantages such as nontoxic, cheap and easy to get, so, α-Fe2O3Material is studied by more and more people in recent years, mesh
Before, nanometer alpha-Fe2O3The preparation method of material has following several: Hydrolyze method, hydro-thermal method, sol-gel method, spray-wall interaction
Method, microemulsion method, the precipitation method, template 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.After this method is by reacting ferrous salt with complexant hydrofluoric acid, ammonium hydroxide is added and adjusts pH value, template is then added
(nearly monodispersed SiO2Or PS sub-micro ball) reaction obtain nanostructure 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 ethyl alcohol and 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；It will mixing
Solution keeps the temperature 6~20 hours formation colloidal sol under the conditions of 20~60 DEG C；Colloidal sol is coated on glass using czochralski method, 30~
60 DEG C drying 0.5~5 hour, formed gel mould；By the gel mould heating on glass, 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.It should
Preparation method, by hydro-thermal method in certain temperature and time, can obtain first using inorganic molysite and acid phosphate as raw material
To favorable dispersibility, 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 mixing, obtains mixed liquor；Trisodium citrate is added in mixed liquor, dissolves it sufficiently after ultrasound, it is molten to obtain faint yellow clarification
Liquid；Resulting faint yellow clear solution is transferred in stainless steel cauldron, temperature reaction；Product after temperature reaction is cooling
To room temperature, will be washed after the centrifuge separation of bottom sediment, products therefrom is dry to get 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 it is added in liquid
Urea obtains faint yellow clear solution；Finally resulting faint yellow clear solution is transferred in reaction kettle, seal and is heated up is anti-
It answers, after product is cooled to room temperature, will be washed after the centrifuge separation of bottom sediment, it is dry to get three-dimensional flower-shaped α type three oxidation 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 acquired product is that three-dimensional spherical, flower-shaped di-iron trioxide or di-iron trioxide are thin
Film.
Summary of the invention
The problem of the purpose of the present invention is to solve prior art preparation complex technical process and high production cost, 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, comprising the following steps:
Step 1: Iron(III) chloride hexahydrate is taken to be placed in alumina crucible, the Iron(III) chloride hexahydrate loadings with
Volume metering is 0.1-0.5 times of alumina crucible total volume, and alumina crucible is then put into the tube furnace equipped with alundum tube
In, both ends sealing；
Step 2: being passed through inert gas into tube furnace, and it is warming up to 380-450 DEG C under protecting under an inert gas, protects
It holds 8-24 hours, then cools to room temperature；
Step 3: the product taken out in alumina crucible is washed through deionized water, after drying, two-dimensional nano piece form is obtained
α-Fe2O3Material.
Further, the alumina crucible equipped with Iron(III) chloride hexahydrate is with cover, and be placed in the tube furnace of alundum tube
Center.
Preferably, the inert gas in the step 2 is one or more 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, it is anti-to thermally decompose oxidation with Iron(III) chloride hexahydrate reagent under inert atmosphere protection by the present invention
Two-dimensional nano piece form α-Fe should be prepared2O3Material, used reagent price is cheap, and preparation process is easier, it can be achieved that scale
Change preparation, and obtained di-iron trioxide pattern is two-dimensional nano piece.
Detailed description of the invention
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.
Specific embodiment
The invention will be further described combined with specific embodiments below, in the illustrative examples and explanation of the invention
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 packed into the alumina crucible of 50 mL, alumina crucible covers
Afterwards, it is put into the tube furnace equipped with alundum tube, after the sealing of tube furnace both ends, is passed through nitrogen purging 10 with 100 mL/min flows
Minute, 380 DEG C then are warming up to 5 DEG C/min rate, and kept for 24 hours, then cooled to room temperature, takes out aluminium oxide earthenware
Product in crucible obtains two-dimensional nano piece form α-Fe after deionized water washing, dry2O3Material, will be made from embodiment 1
Two-dimensional nano piece form α-Fe2O3Material characterizes obtain SEM photograph under a scanning electron microscope, as shown in Figure 1, can from Fig. 1
To find out α-Fe made from the present embodiment2O3Material, pattern be two-dimensional nano piece, about 100 ~ 500 nm of thickness, and accumulate it is tighter
It is close, then as to two-dimensional nano piece form α-Fe made from embodiment 12O3Material carries out X-ray diffraction, analyzes its diffracting spectrum,
As shown in figure 5, obtaining diffraction maximum corresponds 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 packed into the alumina crucible of 50 mL, alumina crucible covers
Afterwards, it is put into the tube furnace equipped with alundum tube, after the sealing of tube furnace both ends, is passed through nitrogen purging 10 with 100 mL/min flows
Minute, 400 DEG C then are warming up to 10 DEG C/min rate, and kept for 20 hours, then cooled to room temperature, takes out aluminium oxide earthenware
Product in crucible obtains two-dimensional nano piece form α-Fe after deionized water washing, dry2O3Material, will be made from embodiment 2
Two-dimensional nano piece form α-Fe2O3Material characterizes obtain SEM photograph under a scanning electron microscope, as shown in Fig. 2, can from Fig. 2
To find out α-Fe made from the present embodiment2O3Material, pattern be two-dimensional nano piece, about 200 ~ 400 nm of thickness, and accumulate it is tighter
It is close.
Embodiment 3
10 mL Iron(III) chloride hexahydrate solid particles will be packed into the alumina crucible of 50 mL, alumina crucible covers
Afterwards, it is put into the tube furnace equipped with alundum tube, after the sealing of tube furnace both ends, is passed through nitrogen purging 10 with 200 mL/min flows
Minute, 420 DEG C then are warming up to 10 DEG C/min rate, and kept for 12 hours, then cooled to room temperature, takes out aluminium oxide earthenware
Product in crucible obtains two-dimensional nano piece form α-Fe after deionized water washing, dry2O3Material, will be made from embodiment 3
Two-dimensional nano piece form α-Fe2O3Material characterizes obtain SEM photograph under a scanning electron microscope, as shown in figure 3, can from Fig. 3
To find out α-Fe made from the present embodiment2O3Material, pattern be two-dimensional nano piece, about 80 ~ 100 nm of thickness, and accumulate it is more loose
It dissipates.
Embodiment 4
5 mL Iron(III) chloride hexahydrate solid particles will be packed into the alumina crucible of 50 mL, after alumina crucible covers,
It is put into the tube furnace equipped with alundum tube, after the sealing of tube furnace both ends, is passed through nitrogen with 200 mL/min flows and purges 10 points
Then clock is warming up to 450 DEG C with 10 DEG C/min rate, and is kept for 8 hours, then cool to room temperature, and takes out alumina crucible
In product after deionized water washing, dry, obtain two-dimensional nano piece form α-Fe2O3Material, will be two made from embodiment 4
Tie up nanometer sheet form α-Fe2O3Material characterizes obtain SEM photograph under a scanning electron microscope, as shown in figure 4, can be with from Fig. 4
Find out α-Fe made from the present embodiment2O3Material, pattern be two-dimensional nano piece, about 100 ~ 800 nm of thickness, and accumulate it is more loose
It dissipates.
The limitation that technical solution of the present invention is not limited to the above specific embodiments, it is all to do according to the technique and scheme of the present invention
Technology deformation out, falls within the scope of protection of the present invention.
Claims (1)
1. a kind of two-dimensional nano piece form α-Fe2O3The preparation method of material, which comprises the following steps:
Step 1: Iron(III) chloride hexahydrate is taken to be placed in alumina crucible with cover, the Iron(III) chloride hexahydrate loadings
Cubing is 0.1-0.5 times of alumina crucible total volume, and alumina crucible is then put into the tubular type equipped with alundum tube
Furnace center, both ends sealing；
Step 2: be passed through inert gas into tube furnace, inert gas is one or more of nitrogen, helium, argon gas,
Gas flow is warming up to 380-450 DEG C in 100-200 mL/min, and under protecting under an inert gas, heating rate 5-10
DEG C/min, it is kept for 8-24 hours, is then cooled to room temperature；
Step 3: the product taken out in alumina crucible is washed through deionized water, after drying, two-dimensional nano piece form α-is obtained
Fe2O3Material.
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| Title |
|---|
| Crystal shape and orientation controlled α-Fe2O3 nanoparticles prepared by decarbonation of FeCO3;Jun Wang et al.;《Modern Physics Letters B》;20140709;第28卷(第18期);1450147 * |
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