CN105129865A - Magnetic micro-nano sheet, and preparation method and application thereof - Google Patents

Magnetic micro-nano sheet, and preparation method and application thereof Download PDF

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CN105129865A
CN105129865A CN201510519389.5A CN201510519389A CN105129865A CN 105129865 A CN105129865 A CN 105129865A CN 201510519389 A CN201510519389 A CN 201510519389A CN 105129865 A CN105129865 A CN 105129865A
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nano
magnetic
alkali
sheet
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CN105129865B (en
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童国秀
刘云
吕天喜
吴文华
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Zhejiang Normal University CJNU
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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)
    • 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
    • C01G49/08—Ferroso-ferric oxide (Fe3O4)
    • 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
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness 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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  • Inorganic Chemistry (AREA)
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Abstract

The invention discloses a magnetic micro-nano sheet, and a preparation method and an application thereof. The magnetic micro-nano sheet is a dimension-adjustable alpha-Fe2O3 or Fe3O4 micro-nano sheet with good dispersion and homogeneity. The alpha-Fe2O3 micro-nano sheet is prepared through a mixed solvent thermal technology, and the dimension and the morphology of the micro-nano sheet are regulated through changing the volume of water, the reactant concentration, a molar ratio of an alkali to a metal salt and the type of the alkali (the diameter of a hexagonal or subround nano-sheet is 60-510nm, and the thickness of the hexagonal or subrotund nano-sheet is 8-30nm; and the diameter of an irregular micro-sheet is 2-16[mu]m, and the thickness of the irregular micro-sheet is 0.35-1[mu]m). The alpha-Fe2O3 is converted into the Fe3O4 micro-nano sheet with strong magnetism and excellent microwave absorption performance through a carbon thermal reduction process. The preparation method has the advantages of no need of a surfactant, simple preparation process, cheap and easily available raw materials, low cost, high output, and easy industrial application and popularization. The micro-nano sheet provided by the invention has application prospects in fields of photocatalysis, microwave absorption, electrode materials, magnetic record materials, sensors and biomedical engineering.

Description

Micro-nano of magnetic and preparation method thereof and application
Technical field
The present invention relates to magnetic Nano technical field, be specifically related to a kind of simple and easy, controlled method preparing micro-nano of magnetic.
Background technology
α-Fe 2o 3and Fe 3o 4because it is stable, low toxicity, rich reserves, the characteristic such as cheap, and become the oxide compound of most important two class iron.α-Fe 2o 3be a kind of n-type semiconductor, its energy gap is 2.1V, has potential application widely in mineral dye, catalyzer, electrode materials, sensor field.Fe 3o 4a kind of traditional magneticsubstance, the Fe of nanoscale 3o 4there is the size electricity relevant with pattern and magnetic performance, as single magnetic domain characteristic, coercivity dimensional change, lower Curie temperature and superparamagnetism, it is made to have a wide range of applications and potential using value in fields such as magnetic recording, microwave absorbing, sensor, bioseparation, biological diagnosis, target administrations.Thus, α-Fe 2o 3and Fe 3o 4controlled synthesis and applied research there is important science and practical significance, enjoy the concern of domestic and international researchist.
Two-dimensional nano sheet has novel optical, electrical, magnetic property because of the shape anisotropy of its uniqueness.Thus developing green, method that is simple, efficient, low cost prepare good dispersity, size, composition the is adjustable micro-nano study hotspot becoming current chemistry and Material Field.
The method of the oxide nano-slice of synthesis iron mainly contains high temperature pyrolytic cracking (HTP), ball milled, coprecipitation method and microwave method.Patent documentation (CN101560695A) discloses a kind of high temperature pyrolytic cracking (HTP) and prepares binary magnetic oxide single crystal nanoplate, the method be by dissolving metal salts in Diethylene Glycol, method by controlling backflow in 140 ~ 190 DEG C of oil bath pans controls reaction, single crystal nanoplate is obtained again through 500 degree of annealing, the organic solvent that the method use cost is higher, the nanometer sheet homogeneity of preparation is poor, react wayward, and the saturation magnetization of products therefrom is lower.Patent documentation (CN104174855A) discloses a kind of tensio-active agent, organism assists ball milling legal system for magnetic Nano sheet, the method is easy to realize a large amount of production, but the ball milling cycle is grown, employ as higher in the cost such as oleic acid, oleyl amine, that non-ambient is friendly tensio-active agent and organic solvent, and the post-processed of product is more complicated, is difficult to obtain clean product.Patent documentation (CN104341010A) discloses a kind of coprecipitation method and prepares SPIO nanometer sheet, the method is simple, easy to operate, gained particle dispersion and homogeneity are better, but the crystallinity of product and saturation magnetization lower, the size adjustable scope of particle is little.Patent documentation (CN101717122A) discloses a kind of preparing ferroferric oxide nano-piece through microwave method, the method is simple, efficient, but employ tensio-active agent, and prepared product is the flower of nanometer sheet composition, but not single dispersing ferroferric oxide nano-piece.
In the present invention, without the need to tensio-active agent, only adopt cheap water and ethanol as solvent, by the hot legal system of mixed solvent for dispersed and that homogeneity is good α-Fe 2o 3micro-nano, and change the amount of water, reactant concn, the ratio of alkali and metal-salt amount of substance, the type of alkali can regulate and control the size of micro-nano on a large scale, gained nanometer sheet has good photocatalysis performance.α-Fe 2o 3micro-nano can change the Fe of ferromagnetism and microwave absorbing property excellence into by protection of inert gas carbo-thermal process 3o 4micro-nano.Prepared micro-nano also has wide potential application foreground by fields such as electrode materials, magnetic recording material, sensor and biomedical engineerings.
Summary of the invention
Technical problem to be solved by this invention is: provide a kind of dispersed and homogeneity good, the preparation method that the magnetic that size, pattern and composition are adjustable is micro-nano.Preparation flow of the present invention is simple, cost is low, output is high, be easy to industrial application promotes; Micro-nano of gained has stronger magnetic responsiveness.
The present invention solves its technical problem and adopts following technical scheme:
Micro-nano provided by the invention, it is α-Fe 2o 3or Fe 3o 4micro-nano.
Above-mentioned α-Fe provided by the invention 2o 3micro-nano, it adopts the hot legal system of mixed solvent standby, specifically: first join in polytetrafluoroethyllining lining by molysite, water and dehydrated alcohol by certain stoichiometric ratio, stirs 5 ~ 10min; Alkali is joined mix and blend 30min in liner again, then liner is put into stainless steel still at 150 ~ 200 DEG C of reaction 6 ~ 12h, cool rear water and dehydrated alcohol centrifuge washing, obtain micro-nano of described good dispersity finally by drying; Described molysite, water, dehydrated alcohol and alkali with magnitude relation be: molysite is 2 ~ 8mmol; Alkali is 5 ~ 20 with the ratio of metal-salt amount of substance; Water is 1.0 ~ 25.0mL, and the cumulative volume of water and dehydrated alcohol is 40.0mL.
Described molysite is one or more in Iron trichloride hexahydrate, Anhydrous Ferric Chloride, nine water iron nitrates.
Described alkali is the one in sodium acetate, sodium carbonate, sodium hydroxide.
Described α-Fe 2o 3micro-nano, it is characterized in that when taking sodium acetate as alkali, the α-Fe of gained 2o 3for the nanometer sheet of monodispersity and the good hexagon of homogeneity or quasi-circular, its diameter is 60 ~ 510nm, and thickness is 8 ~ 30nm; When taking sodium carbonate as alkali, the α-Fe of gained 2o 3for irregular nanometer sheet, its diameter is 180 ~ 210nm, and thickness is 18 ~ 21nm; When taking sodium hydroxide as alkali, the α-Fe of gained 2o 3for the irregular micron film of good dispersity, its diameter is 2 ~ 16 μm, and thickness is 0.35 ~ 1 μm.
α-the Fe that the hot legal system of above-mentioned employing mixed solvent is standby 2o 3micro-nano, its application in catalyzer, electrode materials, mineral dye or sensor.
The preparation method that described magnetic is micro-nano, with above-mentioned α-Fe 2o 3micro-nano, as precursor, adopts protection of inert gas carbo-thermal process to prepare scattered Fe 3o 4micro-nano, specifically: by above-mentioned for 0.2g micro-nano and 1.0 ~ 3.0mL benzene or acetone at 400 ~ 500 DEG C, thermal treatment 2h under nitrogen or argon gas atmosphere, the heating-up time is 1h, obtains the Fe that magnetic is stronger 3o 4micro-nano.
Described Fe 3o 4micro-nano saturation magnetization is 82.51 ~ 89.50emu/g.
Fe prepared by above-mentioned employing protection of inert gas carbo-thermal process 3o 4micro-nano, its application in catalyzer, electrode materials, microwave absorption, high density magnetic recording material or sensor.
The present invention, owing to have employed above-mentioned technical scheme, makes it compared with prior art, has following advantage and positively effect:
(1) α-Fe that provides of present method 2o 3and Fe 3o 4micro-nano has dispersed and homogeneity is good, and size range is wide, and (hexagonal nanosheet grows 60 ~ 510nm, thick about 8 ~ 30nm; Irregular micron film 2 ~ 16 μm, thick about 0.35 ~ 1 μm) etc. characteristic.
(2) present method is without the need to tensio-active agent, green high-efficient.Raw materials used cheap and easy to get, preparation cost is low.
(3) present method preparation process is simple, reproducible.
(4) application is wide: micro-nano of the magnetic provided has excellent photocatalysis performance, strong magnetic response and microwave absorbing property, will have broad application prospects in fields such as catalyzer, electrode materials, microwave absorbing, magnetic recording material, sensor and biomedical engineerings.
Accompanying drawing explanation
The thing phase that Fig. 1 ~ Fig. 2 is respectively embodiment 1 products therefrom and the pattern observed under scanning electron microscope.
Fig. 3 ~ Figure 14 is respectively the pattern that embodiment 2 ~ embodiment 13 products therefrom observes under scanning electron microscope.
Figure 15 ~ Figure 16 is respectively the ultraviolet-visible collection of illustrative plates of rhodamine B solution under embodiment 1 and the effect of embodiment 4 products therefrom.
Figure 17 ~ Figure 19 is respectively the thing phase of embodiment 14 products therefrom, the pattern observed under scanning electron microscope and electrostatic theory figure.
The thing phase that Figure 20 ~ Figure 21 is respectively embodiment 15 products therefrom and the pattern observed under scanning electron microscope.
Figure 22 ~ Figure 27 is respectively the pattern that embodiment 16 ~ embodiment 21 products therefrom observes under scanning electron microscope.
Figure 28 ~ Figure 31 is respectively the thing phase of embodiment 22 products therefrom, the pattern observed under scanning electron microscope, electrostatic theory figure and reflection loss curve.
Embodiment
The present invention adopts the hot method of mixed solvent, and by changing the volume of water and dehydrated alcohol, reactant concn, alkali regulates and controls α-Fe with the ratio of metal-salt amount of substance, the type of alkali 2o 3the size of micro-nano.And α-Fe 2o 3sheet can change ferromagnetic Fe into further by protection of inert gas carbo-thermal process 3o 4micro-nano.Micro-nano of gained has dispersed and homogeneity is good and the characteristic such as size adjustable.
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, but be not only confined to the following examples.
Embodiment 1:
By 4mmolFeCl 36H 2o, 3.0mL distilled water, 37.0mL dehydrated alcohol are added in polytetrafluoroethyllining lining, and magnetic agitation 5min, obtains clear solution.40mmol sodium acetate (alkali is 10 with the ratio of metal-salt amount of substance) is joined mix and blend 30min in liner.Finally liner is put into stainless steel still at 180 DEG C of reaction 12h, centrifuge washing after cooling.60 DEG C of dry 6h obtain required dispersed nano sheet.Products therefrom is brick-red, and the thing phase of product, the pattern that observes under scanning electron microscope are respectively as shown in Figure 1-2.Visible, product is hexagon α-Fe 2o 3nanometer sheet, its diameter (for the external circular diameter of hexagon) is 121 ~ 173nm, and thickness is about 10nm.
Take 10mg sample in 100 milliliters of small beakers, measure 50mL0.02mmol/L rhodamine B solution, pour in above-mentioned small beaker, under dark condition, stir 30min, then in small beaker, add 0.255mL30%H 2o 2solution, under small beaker being placed in 300W xenon lamp, illumination magnetic agitation reacts 120min again, and at different time (0min, 10min, 20min, 40min, 70min, 120min) get the centrifugation of 4mL reaction solution, get supernatant liquor, finally utilize ultraviolet-visible spectrophotometer to survey the ultraviolet-visible spectrum of solution as shown in figure 15.
Embodiment 2:
Identical with embodiment 1 step, but distilled water is 1.0mL, and dehydrated alcohol is 39.0mL.Products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in Figure 3, visible, and the minimizing of the water yield causes α-Fe 2o 3the diameter of hexagonal nanosheet increases to 355 ~ 868nm, and thickness is about 30nm.
Embodiment 3:
Identical with embodiment 1 step, but distilled water is 4.0mL, and dehydrated alcohol is 36.0mL.Products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in Figure 4, visible, and the increase of the water yield causes α-Fe 2o 3the diameter of hexagonal nanosheet is decreased to 83 ~ 120nm, and thickness is about 15nm.
Embodiment 4:
Identical with embodiment 1 step, but distilled water is 8.0mL, and dehydrated alcohol is 32.0mL.Products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in Figure 5, visible, and the further increase of the water yield causes α-Fe 2o 3the diameter of hexagonal nanosheet is decreased to 48 ~ 68nm.The ultraviolet-visible light spectrogram of rhodamine B solution different irradiation time under catalyst action as shown in figure 16.
Embodiment 5:
Identical with embodiment 1 step, but sodium acetate is 20mmol (alkali is 5 with the ratio of metal-salt amount of substance).Products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in Figure 6, visible, and alkali causes α-Fe with the reduction of the ratio of metal-salt amount of substance 2o 3the diameter of hexagonal nanosheet is decreased to 58 ~ 96nm.
Embodiment 6:
Identical with embodiment 1 step, but sodium acetate is 80mmol (alkali is 20 with the ratio of metal-salt amount of substance).Products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in Figure 7, visible, and alkali causes α-Fe with the increase of the ratio of metal-salt amount of substance 2o 3the diameter of hexagonal nanosheet is increased to 250 ~ 350nm, and thickness is about 8nm.
Embodiment 7:
Identical with embodiment 1 step, but alkali is anhydrous sodium carbonate.Products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in Figure 8, visible, and product is irregular α-Fe 2o 3nanometer sheet, it is 180 ~ 210nm that nanometer sheet is about, and thickness is 18 ~ 21nm.
Embodiment 8:
Identical with embodiment 1 step, but FeCl 36H 2o is 2mmol, and sodium acetate is 20mmol, and products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in Figure 9, visible, and the reduction of iron salt concentration causes hexagon α-Fe 2o 3the diameter of nanometer sheet is reduced to 103 ~ 141nm.
Embodiment 9:
Identical with embodiment 1 step, but FeCl 36H 2o is 8mmol, and sodium acetate is 80mmol, and products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in Figure 10, visible, and the increase of iron salt concentration causes hexagon α-Fe 2o 3the diameter of nanometer sheet is increased to 220 ~ 281nm.
Embodiment 10:
Identical with embodiment 1 step, but molysite is Fe (NO 3) 39H 2o.Products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in figure 11, visible, and product is hexagonal α-Fe 2o 3nanometer sheet, nanometer sheet diameter is 126 ~ 171nm, and thickness is about 20nm.
Embodiment 11:
Identical with embodiment 1 step, but molysite is anhydrous FeCl 3.Products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in figure 12, visible, and product is hexagonal α-Fe 2o 3nanometer sheet, nanometer sheet diameter is 174 ~ 225nm, and thickness is about 20nm.
Embodiment 12:
Identical with embodiment 1 step, but temperature of reaction is 150 DEG C.Products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in figure 13, visible, and product is rotund α-Fe 2o 3nanometer sheet, nanometer sheet surface adsorption complete nanocrystalline of a large amount of unreacted, and nanometer sheet diameter is 139 ~ 160nm, and thickness is about 25nm.
Embodiment 13:
Identical with embodiment 12 step, but temperature of reaction is 200 DEG C.Products therefrom is brick-red, and the pattern observed under scanning electron microscope is as shown in figure 14, visible, and product is rotund α-Fe 2o 3nanometer sheet, nanometer sheet diameter is 124 ~ 165nm, and thickness is about 20nm.
Embodiment 14:
By gained sample in 0.2 gram of embodiment 1, load with the ceramic Noah's ark of 6cm × 3cm × 1.5cm, in Noah's ark, add 3 milliliters of acetone, Noah's ark is placed in single warm tube furnace, in 400 DEG C of reactions, 1 hour (heating-up time is 1 hour) under argon shield.Reaction terminate after under argon shield furnace cooling to room temperature.The thing phase of products therefrom, the pattern that observes under scanning electron microscope are respectively as shown in Figure 17 ~ Figure 18, and visible, calcining after product is hexagon Fe 3o 4nanometer sheet.The 7404 type vibrating sample magnetometers adopting LakeShore company of the U.S. to produce record the electrostatic theory of product as shown in figure 19, and its saturation magnetization is 82.51emu/g, and coercive force is 256.56Oe, and remanent magnetism is 26.00emu/g.
Embodiment 15:
Identical with embodiment 1 step, but alkali is sodium hydroxide.Products therefrom is the atropurpureus of light, and the thing phase of product, the pattern that observes under scanning electron microscope are respectively as shown in Figure 20 ~ Figure 21, and visible, product is irregular α-Fe 2o 3micron film, sheet diameter is 5 ~ 17 μm, and thickness is about 0.75 μm.
Embodiment 16:
Identical with embodiment 15 step, but distilled water is 15.0mL, and dehydrated alcohol is 25.0mL.Products therefrom is the atropurpureus of light, and the pattern observed under scanning electron microscope is as Figure 22, visible, and product is irregular α-Fe 2o 3micron film, sheet diameter is 3 ~ 12 μm, and thickness is about 0.75 μm.
Embodiment 17:
Identical with embodiment 15 step, but distilled water is 25.0mL, and dehydrated alcohol is 15.0mL.Products therefrom is the atropurpureus of light, and the pattern observed under scanning electron microscope is as Figure 23, visible, and product is irregular α-Fe 2o 3micron film, there is more small-particle on sheet surface, and diameter is 0.79 ~ 3.1 μm, and thickness is about 0.35 μm.
Embodiment 18:
Identical with embodiment 15 step, but temperature of reaction is 150 DEG C.Products therefrom is the atropurpureus of light, and the pattern observed under scanning electron microscope is as Figure 24, visible, and product is irregular α-Fe 2o 3micron film, there is more floss on sheet surface, and diameter is 7 ~ 20 μm, and thickness is about 1 μm.
Embodiment 19:
Identical with embodiment 15 step, but temperature of reaction is 200 DEG C.Products therefrom is the atropurpureus of light, and the pattern observed under scanning electron microscope is as Figure 25, visible, and product is irregular α-Fe 2o 3micron film, sheet diameter is 10 ~ 24 μm, and thickness is about 1 μm.
Embodiment 20:
Identical with embodiment 8 step, but alkali is sodium hydroxide.Products therefrom is the atropurpureus of light, and respectively as shown in figure 26, visible, product is irregular α-Fe to the pattern observed under scanning electron microscope 2o 3the flower of micron film or micron film composition, sheet diameter is 9 ~ 16 μm, and thickness is about 0.8 μm.
Embodiment 21:
Identical with embodiment 15 step, but the reaction times be 6 hours.Products therefrom is the black of light, and the pattern observed under scanning electron microscope is as shown in figure 27, visible, and product is irregular α-Fe 2o 3micron film, sheet diameter is 11 ~ 22 μm, and thickness is about 0.8 μm.
Embodiment 22:
By gained sample in 0.2 gram of embodiment 15, load with the ceramic Noah's ark of 6cm × 3cm × 1.5cm, in Noah's ark, add 1 milliliter of benzene, Noah's ark is placed in single warm tube furnace, under nitrogen protection in 500 DEG C of reactions 2h (heating-up time is 1h).Reaction terminate after under nitrogen protection furnace cooling to room temperature.The thing phase of products therefrom, the pattern that observes under scanning electron microscope are respectively as shown in Figure 28 ~ Figure 29, and visible, calcining after product pattern does not change, and is irregular Fe 3o 4micron film.As shown in figure 30, its saturation magnetization is 89.50emu/g to the electrostatic theory figure of product, and coercive force is 238.54Oe, and remanent magnetism is 22.50emu/g.Be the Fe of 60% by massfraction 3o 4nanometer sheet/paraffin matrix material is pressed into the coaxial sample of internal diameter 3mm, external diameter 7mm, high about 3.5mm, tests its Micro-wave low-noise transistor, then use at Agilent 5230A network vector analyser formulae discovery microwave reflection rate, reflection loss curve as shown in figure 31.Be less than-20dB in 6.0 – 16.8GHz range of frequency internal reflection rates, maximum reflection loss is-32.5dB.

Claims (9)

1. micro-nano an of magnetic, it is characterized in that described micro-nano consist of α-Fe 2o 3or Fe 3o 4.
2. a preparation method for micro-nano of magnetic, is characterized in that a kind of α-Fe adopting the hot legal system of mixed solvent standby 2o 3micro-nano, specifically: first join in polytetrafluoroethyllining lining by molysite, water and dehydrated alcohol by certain stoichiometric ratio, stir 5 ~ 10min; Alkali is joined mix and blend 30min in liner again, then liner is put into stainless steel still at 150 ~ 200 DEG C of reaction 6 ~ 12h, cool rear water and dehydrated alcohol centrifuge washing, obtain micro-nano of described good dispersity finally by drying;
Described molysite, water, dehydrated alcohol and alkali with magnitude relation be: molysite is 2 ~ 8mmol; Alkali is 5 ~ 20 with the ratio of metal-salt amount of substance; Water is 1.0 ~ 25.0mL, and the cumulative volume of water and dehydrated alcohol is 40.0mL.
3. the preparation method of micro-nano of magnetic as claimed in claim 2, is characterized in that molysite is one or more in Iron trichloride hexahydrate, Anhydrous Ferric Chloride, nine water iron nitrates.
4. the preparation method of micro-nano of magnetic as claimed in claim 2, is characterized in that alkali is the one in sodium acetate, sodium carbonate, sodium hydroxide.
5. the preparation method of micro-nano of magnetic as claimed in claim 2, is characterized in that when taking sodium acetate as alkali, the α-Fe of gained 2o 3for the nanometer sheet of monodispersity and the good hexagon of homogeneity or quasi-circular, its diameter is 60 ~ 510nm, and thickness is 8 ~ 30nm; When taking sodium carbonate as alkali, the α-Fe of gained 2o 3for irregular nanometer sheet, its diameter is 180 ~ 210nm, and thickness is 18 ~ 21nm; When taking sodium hydroxide as alkali, the α-Fe of gained 2o 3for the irregular micron film of good dispersity, its diameter is 2 ~ 16 μm, and thickness is 0.35 ~ 1 μm.
6. α-the Fe that in claim 2 ~ 5 prepared by method described in arbitrary claim 2o 3micro-nano, its application in catalyzer, electrode materials, mineral dye or sensor.
7. a preparation method for micro-nano of magnetic, is characterized in that the α-Fe with claim 3 ~ 5 gained 2o 3micro-nano, as precursor, adopts protection of inert gas carbo-thermal process to prepare Fe 3o 4micro-nano, specifically: by the α-Fe of 0.2g 2o 3micro-nano, 1.0 ~ 3.0mL benzene or acetone at 400 ~ 500 DEG C, thermal treatment 2h under nitrogen or argon gas atmosphere, the heating-up time is 1h, obtains the Fe that magnetic is stronger 3o 4micro-nano.
8. the preparation method of micro-nano of magnetic as claimed in claim 7, is characterized in that described Fe 3o 4micro-nano, its saturation magnetization range is 82.51 ~ 89.50emu/g.
9. the Fe that in claim 7 ~ 8, described in arbitrary claim prepared by method 3o 4micro-nano, its application in catalyzer, electrode materials, microwave absorption, high density magnetic recording material or sensor.
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