CN108439482A - A kind of grain size and the adjustable magnetism α-Fe of pattern2O3The preparation method of nano-powder - Google Patents
A kind of grain size and the adjustable magnetism α-Fe of pattern2O3The preparation method of nano-powder Download PDFInfo
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- 239000011858 nanopowder Substances 0.000 title claims abstract description 25
- 230000005389 magnetism Effects 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229910000859 α-Fe Inorganic materials 0.000 title claims description 14
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000000843 powder Substances 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- 239000004471 Glycine Substances 0.000 claims abstract description 23
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims abstract description 10
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 230000008025 crystallization Effects 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 229910003145 α-Fe2O3 Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 18
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 abstract description 14
- 239000006185 dispersion Substances 0.000 abstract description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 235000013759 synthetic iron oxide Nutrition 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract 1
- 235000013339 cereals Nutrition 0.000 description 12
- 239000002245 particle Substances 0.000 description 10
- 239000000919 ceramic Substances 0.000 description 9
- 238000009826 distribution Methods 0.000 description 8
- 238000000445 field-emission scanning electron microscopy Methods 0.000 description 6
- 230000005415 magnetization Effects 0.000 description 6
- 239000003643 water by type Substances 0.000 description 6
- 230000006698 induction Effects 0.000 description 4
- 239000002351 wastewater Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 3
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000975 dye Substances 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 235000013312 flour Nutrition 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000005642 Oleic acid Substances 0.000 description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 229910001566 austenite Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000004907 flux Effects 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- NKJOXAZJBOMXID-UHFFFAOYSA-N 1,1'-Oxybisoctane Chemical compound CCCCCCCCOCCCCCCCC NKJOXAZJBOMXID-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000190070 Sarracenia purpurea Species 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- MHDVGSVTJDSBDK-UHFFFAOYSA-N dibenzyl ether Chemical compound C=1C=CC=CC=1COCC1=CC=CC=C1 MHDVGSVTJDSBDK-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- UYPYRKYUKCHHIB-UHFFFAOYSA-N trimethylamine N-oxide Chemical compound C[N+](C)(C)[O-] UYPYRKYUKCHHIB-UHFFFAOYSA-N 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]
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01P2004/30—Particle morphology extending in three dimensions
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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
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Catalysts (AREA)
Abstract
The invention discloses the adjustable magnetism α Fe of a kind of grain size and pattern2O3The preparation method of nano-powder, using glycine and crystallization iron chloride as raw material, be added reaction kettle in using after hydro-thermal method by detaching, being dried to obtain magnetic α Fe2O3Nano-powder.Compared with prior art, beneficial effects of the present invention are：The present invention avoids pollution problem by a kind of simple hydro-thermal method synthetic iron oxide nano-powder using glycine, improves production efficiency and cost is relatively low.Acquired powder more stable and uniform, dispersion degree are also more preferable.It obtains as magnetic ferric oxide nano powder, and the dosage for changing glycine is controllable to the pattern and grain size of nano-powder.
Description
Technical field
The present invention relates to the preparing technical field for composite material in terms of environmental wastewater reparation, especially a kind of grain size and
The adjustable magnetism α-Fe of pattern2O3The preparation method of nano-powder.
Background technology
With conventional physical-chemical method cannot be fully effective processing waste water from dyestuff, people pass through study find
Photochemical catalytic oxidation can make waste water from dyestuff redox at harmless substance.Therefore, photocatalysis treatment waste water from dyestuff causes people
Attention.Magnetic Nano ferric oxide particles size is small, large specific surface area, can increase connecing for catalysis reaction as catalyst carrier
Contacting surface is accumulated, and keeps catalytic performance more notable.
Hyeon etc. is by under the conditions of 100 DEG C, by Fe (CO)5It is added in the mixture of Octyl Ether and oleic acid and is divided
Then trimethylamine oxide is added as weak oxidant in solution, temperature rising reflux 1h prepares the monodispersed γ-Fe of 11nm or so2O3
Nano particle.The FeCl such as Woo3·6H2It is micro- to form water-in-oil type in the benzyl oxide for making surfactant with oleic acid for O aqueous dispersions
Lotion.Then, propylene is added as proton consumption agent, obtains Fe2O3Gel；Wang Yinghui etc. is forerunner with ethylene glycol and ferric nitrate
Object, 70 DEG C are heated to reflux generation colloidal sol, and 80 DEG C of heating water baths obtain xerogel, and γ-Fe are prepared in last calcination2O3Particle；Zhao
Deng using ammonium hydroxide as precipitating reagent and controlling the pH value of solution, Fe is adjusted2+And Fe3+Substance amount ratio be 1.75:1, it is protected in argon gas
Under synthesize magnetic Fe3O4Nano particle.In magnetic Nano material field, had been carried out for various types of iron oxide
Many researchs, and the research that magnetic iron oxide is prepared for glycine is fewer and fewer.
Invention content
The object of the present invention is to provide the adjustable magnetism α-Fe of a kind of grain size and pattern2O3The preparation method of nano-powder, with
Solve deficiency in the prior art.
The present invention provides the adjustable magnetism α-Fe of a kind of grain size and pattern2O3The preparation method of nano-powder, including it is following
Step：
（1）Glycine and crystallization iron chloride are taken, beaker is poured into, deionized water is added as solvent, is placed in magnetic agitation
It is stirred on device, obtains yellow solution；
（2）By step（1）In yellow solution pour into advance washed hydrothermal reaction kettle, then beaker is rushed with deionized water
It is poured into reaction kettle after washing, reaction kettle is covered and is put into constant temperature convection oven, reaction temperature and reaction time are set, wait reacting
After take out reaction kettle；
（3）By the powder centrifuge of generation, and absolute ethyl alcohol and deionized water is used alternately to wash for several times respectively, will washed
Powder, which is put into vacuum drying chamber, afterwards is dried to obtain micromagnetism rufous α-Fe2O3Powder.
Preferably, step（1）Described in mass ratio between glycine and iron chloride be 1~5：1.
Preferably, step（2）Described in reaction temperature be 180~200 DEG C, the reaction time be 6~48 h.
Preferably, step（3）The drying temperature of the middle drying box used is 20~60 DEG C, and drying time is 4~12
h。
Compared with prior art, beneficial effects of the present invention are：The present invention passes through a kind of simple hydro-thermal method synthetic iron oxide
Nano-powder avoids pollution problem using glycine, improves production efficiency and cost is relatively low.Acquired powder is more stablized
Uniformly, dispersion degree is also more preferable.It obtains as magnetic ferric oxide nano powder, and changes pattern of the dosage to nano-powder of glycine
It is controllable with grain size.
Description of the drawings
Fig. 1 a are α-Fe prepared by embodiment 12O3The field emission scanning electron microscope of nano-powder（FE-SEM）Figure；Obtained by Fig. 1 b
The particle frequency distribution map of powder；The XRD diagram of powder obtained by Fig. 1 c；The magnetization curve of powder obtained by Fig. 1 d.
Fig. 2 a are α-Fe prepared by embodiment 22O3The field emission scanning electron microscope of nano-powder（FE-SEM）Figure；Obtained by Fig. 2 b
The particle frequency distribution map of powder；The XRD diagram of powder obtained by Fig. 2 c；The magnetization curve of powder obtained by Fig. 2 d.
Fig. 3 a are α-Fe prepared by embodiment 32O3The field emission scanning electron microscope of nano-powder（FE-SEM）Figure；Obtained by Fig. 3 b
The particle frequency distribution map of powder；The XRD diagram of powder obtained by Fig. 3 c；The magnetization curve of powder obtained by Fig. 3 d.
Specific implementation mode
The embodiments described below with reference to the accompanying drawings are exemplary, is only used for explaining the present invention, and cannot be construed to
Limitation of the present invention.
A kind of grain size and the adjustable magnetism α-Fe of pattern2O3The preparation method of nano-powder, includes the following steps：
（1）Glycine and crystallization iron chloride are taken, beaker is poured into, deionized water is added as solvent, is placed in magnetic agitation
It is stirred on device, obtains yellow solution；The step is intended to obtain the precursor of ferric iron and glycine.
（2）By step（1）In yellow solution pour into advance washed hydrothermal reaction kettle, then will be burnt with deionized water
Cup pours into after rinsing in reaction kettle, and reaction kettle is covered and is put into constant temperature convection oven, and reaction temperature and reaction time is arranged, waits for
Reaction kettle is taken out after reaction；The step is intended under hydrothermal conditions, and the precursor of ferric iron and glycine divides in situ
Solution forms α-Fe2O3 nucleus, and regeneration grows up to the α-Fe2O3 particles of different-grain diameter and pattern.
（3）By the powder centrifuge of generation, and absolute ethyl alcohol and deionized water is used alternately to wash for several times respectively, it will
Powder, which is put into vacuum drying chamber, after washing is dried to obtain micromagnetism rufous α-Fe2O3 powder.
Preferably, step（1）Described in mass ratio between glycine and iron chloride be 1~5：1.
Preferably, step（2）Described in reaction temperature be 180~200 DEG C, the reaction time be 6~48 h.
Preferably, step（3）The drying temperature of the middle drying box used is 20~60 DEG C, and drying time is 4~12
h。
The embodiment of the present invention 1
（1）0.5 g glycine and the crystallization iron chloride of 0.54 g are weighed respectively, is poured into beaker, and 15 mL deionized waters are added
It as solvent, and is placed on magnetic stirring apparatus and stirs 30 min, solution is yellow when stirring.
（2）Liquid will be stirred to pour into advance washed 25mL hydrothermal reaction kettles, then with 5mL deionized waters by beaker
It is poured into reaction kettle after flushing；Reaction kettle is covered and is put into constant temperature convection oven, setting temperature is 200 DEG C, reacts 10h；It waits for
After reaction reaction was completed kettle cooling and after, take out reaction kettle, the powder centrifuge that will be generated after reaction, and use nothing respectively
Alternately for several times, powder after washing is put into vacuum drying chamber for washing for water-ethanol and deionized water, and setting temperature is 40 DEG C, vacuum
Dry 10h obtains micromagnetism iron oxide red brown ceramic powder.Fig. 1 a are that micromagnetism iron oxide red brown ceramic powder prepared by embodiment 1 is received
The field emission scanning electron microscope FE-SEM figures of rice flour body (figure a, b correspond to high and low multiplying power image respectively).As seen from the figure, obtained
Micromagnetism iron oxide red brown ceramic powder nano-powder pattern is mainly two kinds：Polyhedron and bulk, surface show as smooth.Figure
1b gives the particle frequency distribution map of gained powder, and average grain diameter is 91 nm as seen from the figure.Fig. 1 c are the XRD of products therefrom
Collection of illustrative plates, with the comparison of JCPDS (PDF No.33-0664) standard card it is found that experimental product and α-Fe2O3Standard diffraction peak one
It causes.Wherein（104）、（110）、（113）、（024）、（116）、（214）、（300）Crystal face is that spike illustrates α-Fe2O3Crystallization is preferable.
Fig. 1 d give the magnetization curve of product, and by hysteresis loop it is found that when 0.5g glycine is added, saturation induction density is
0.374 emu/g, residual magnetic flux density are 0.029 emu/g, and coercivity is 114.9 Oe.
The embodiment of the present invention 2
（1）1.0g glycine and the crystallization iron chloride of 0.54g are weighed respectively, is poured into beaker, and 15mL deionized waters are added and make
It for solvent, and is placed on magnetic stirring apparatus and stirs 30min, solution is yellow when stirring.
（2）Liquid will be stirred to pour into advance washed 25mL hydrothermal reaction kettles, then with 5mL deionized waters by beaker
It is poured into reaction kettle after flushing；Reaction kettle is covered and is put into constant temperature convection oven, setting temperature is 200 DEG C, reacts 10h；It waits for
After reaction reaction was completed kettle cooling and after, take out reaction kettle, the powder centrifuge that will be generated after reaction, and use nothing respectively
Alternately for several times, powder after washing is put into vacuum drying chamber for washing for water-ethanol and deionized water, and setting temperature is 40 DEG C, vacuum
Dry 10h obtains micromagnetism iron oxide red brown ceramic powder.Fig. 2 a are that micromagnetism iron oxide red brown ceramic powder prepared by embodiment 2 is received
The field emission scanning electron microscope FE-SEM figures of rice flour body.As seen from the figure, obtained micromagnetism iron oxide red brown ceramic powder nano powder
Body is in mainly two kinds of patterns：Spherical and irregular, surface shows as smooth.Fig. 2 b give the particle frequency of gained powder
Distribution map, average grain diameter is 95 nm as seen from the figure.Fig. 2 c are the XRD spectrum of products therefrom, with JCPDS (PDF No.33-
0664) standard card comparison is it is found that experimental product and α-Fe2O3Standard diffraction peak it is consistent.Wherein（104）、（110）、（113）、
（024）、（116）、（214）、（300）Crystal face is that spike illustrates α-Fe2O3Crystallization is preferable.Fig. 2 d give the magnetization curve of product,
By hysteresis loop it is found that when 1.0 g glycine is added, saturation induction density is 0.304 emu/g, and residual magnetic induction is strong
Degree is 0.067 emu/g, and coercivity is 429.5 Oe.
The embodiment of the present invention 3
（1）1.5g glycine and the crystallization iron chloride of 0.54g are weighed respectively, is poured into beaker, and 15mL deionized waters are added and make
It for solvent, and is placed on magnetic stirring apparatus and stirs 30min, solution is yellow when stirring.
（2）Liquid will be stirred to pour into advance washed 25mL hydrothermal reaction kettles, then with 5mL deionized waters by beaker
It is poured into reaction kettle after flushing；Reaction kettle is covered and is put into constant temperature convection oven, setting temperature is 200 DEG C, reacts 10h；It waits for
After reaction reaction was completed kettle cooling and after, take out reaction kettle, the powder centrifuge that will be generated after reaction, and use nothing respectively
Alternately for several times, powder after washing is put into vacuum drying chamber for washing for water-ethanol and deionized water, and setting temperature is 40 DEG C, vacuum
Dry 10h obtains micromagnetism iron oxide red brown ceramic powder.Fig. 3 a are that micromagnetism iron oxide red brown ceramic powder prepared by embodiment 3 is received
The field emission scanning electron microscope FE-SEM figures of rice flour body.As seen from the figure, obtained micromagnetism iron oxide red brown ceramic powder nano powder
Bodily form looks are uniform, and the pattern presented is spherical, and surface is smooth.Fig. 3 b give the particle frequency distribution map of gained powder,
Average grain diameter is 207 nm as seen from the figure.Fig. 3 c are the XRD spectrum of products therefrom, with JCPDS (PDF No.33-0664) standard
Card compares it is found that experimental product and α-Fe2O3Standard diffraction peak it is consistent.Wherein（104）、（110）、（113）、（024）、
（116）、（214）、（300）Crystal face is that spike illustrates α-Fe2O3Crystallization is preferable.Fig. 3 d give the magnetization curve of product, by magnetic hysteresis
For loop line it is found that when 1.5 g glycine is added, saturation induction density is 0.215 emu/g, and residual magnetic flux density is
0.034 emu/g, coercivity are 492.5 Oe.
Gradually increasing with glycine amount, magnetic α-Fe it can be seen from particle size distribution figure and SEM photograph2O3Be averaged
Grain size gradually increases, and its pattern finally converts to polyhedron, more tends to regular from bulk to spherical shape.It can from hysteresis loop
To obtain：With the addition of glycine amount, magnetic α-Fe2O3The grain size of nano-powder gradually increases, magnetic gradually to weaken.
Table 1 is the pattern and size distribution table of embodiment 1-3.
Table 1
| Glycine Levels/g | Product morphology | Average grain diameter/nm |
| 0.5 | It is blocky | 91 |
| 1.0 | It is spherical | 95 |
| 1.5 | Polyhedron | 207 |
The structure, feature and effect of the present invention are described in detail based on the embodiments shown in the drawings, the above is only
For presently preferred embodiments of the present invention, but the present invention is not to limit practical range, every conception institute according to the present invention shown in drawing
The change of work, or it is revised as the equivalent embodiment of equivalent variations, it, should all when not going beyond the spirit of the description and the drawings
Within the scope of the present invention.
Claims (4)
1. a kind of grain size and the adjustable magnetism α-Fe of pattern2O3The preparation method of nano-powder, it is characterised in that：
Glycine and crystallization iron chloride are taken, beaker is poured into, deionized water is added as solvent, is placed on magnetic stirring apparatus
Stirring, obtains yellow solution；
By step（1）In yellow solution pour into advance washed hydrothermal reaction kettle, then beaker is rinsed with deionized water
After pour into reaction kettle, reaction kettle is covered and is put into constant temperature convection oven, reaction temperature and reaction time are set, waits for reaction knot
Reaction kettle is taken out after beam；
By the powder centrifuge of generation, and absolute ethyl alcohol and deionized water is used alternately to wash for several times, after washing respectively
Powder, which is put into vacuum drying chamber, is dried to obtain micromagnetism rufous α-Fe2O3Powder.
2. grain size according to claim 1 and the adjustable magnetism α-Fe of pattern2O3The preparation method of nano-powder, feature
It is：Step（1）Described in mass ratio between glycine and iron chloride be 1~5：1.
3. grain size according to claim 1 and the adjustable magnetism α-Fe of pattern2O3The preparation method of nano-powder, feature
It is：Step（2）Described in reaction temperature be 180~200 DEG C, the reaction time be 6~48 h.
4. grain size according to claim 1 and the adjustable magnetism α-Fe of pattern2O3The preparation method of nano-powder, feature
It is：Step（3）The drying temperature of the middle drying box used is 20~60 DEG C, and drying time is 4~12 h.
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