CN106745305A - A kind of α Fe2O3The preparation method of magnetic nano powder material - Google Patents

A kind of α Fe2O3The preparation method of magnetic nano powder material Download PDF

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Publication number
CN106745305A
CN106745305A CN201611131662.8A CN201611131662A CN106745305A CN 106745305 A CN106745305 A CN 106745305A CN 201611131662 A CN201611131662 A CN 201611131662A CN 106745305 A CN106745305 A CN 106745305A
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powder material
nano powder
magnetic nano
urea
preparation
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刘瑞江
陆荣柱
陈健
陆益民
虞乐群
吴晓阳
于宗良
邓志勇
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Jiangsu University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00Compounds of iron
    • C01G49/02Oxides; Hydroxides
    • C01G49/06Ferric oxide [Fe2O3]
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/42Magnetic properties

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Hard Magnetic Materials (AREA)
  • Compounds Of Iron (AREA)

Abstract

The invention belongs to inorganic nonmetal magnetic Synthesis Teckniques of Nanostructured Powders field, and in particular to a kind of α Fe2O3The preparation method of magnetic nano powder material;The present invention with inorganic molysite and urea as raw material, by Fe3+With urea according to not less than 5:1 mol ratio is dissolved in water, and controls Fe3+The mol/L of concentration 0.5 3.0, stirring is reacted between being warming up to 85 98 DEG C, and reaction terminates rear centrifugation, and is precipitated with distillation water washing, will precipitate drying, grinds, and being placed in temperature programmed control resistance furnace the calcining at 500 700 DEG C can obtain α Fe2O3Magnetic nano powder material.The present invention prepares α Fe using the dispersed source of iron of urea and urea decomposition reaction2O3Magnetic nano powder material, its process is simple, and operation is easy, and low cost is low for equipment requirements, environmental protection, and product structure pattern is uniform, stable performance.

Description

A kind of α-Fe2O3The preparation method of magnetic nano powder material
Technical field
The present invention relates to a kind of α-Fe2O3The preparation method of magnetic nano powder material, belongs to inorganic nonmetallic nanometer material Preparing technical field.
Background technology
Iron is most common and one of the most widely used metal material of production and living, and wherein iron oxide is to be only second to titanium white Powder measures big and wide inorganic pigment in the world, is widely used in military affairs, building materials, catalyst, ceramics, glass, magnetic The industrial chemicals in the fields such as material, papermaking, cosmetics.Di-iron trioxide can be divided into α-Fe according to crystal formation difference2O3、β-Fe2O3With γ-Fe2O3, wherein α-Fe2O3It is brick-red solid powder, is one of the most stable ferriferous oxide under normal temperature, it has anti-corruption Corrosion is strong, good weatherability, low toxicity, it is inexpensive the features such as, be a kind of typical n types semi-conducting material, be widely used in pigment, The fields such as ceramics, catalyst, gas sensor, magnetic material preparation and nano composite material preparation.
From 20th century after the mid-80 scientist successfully develops nano metal material, scientist begins to study nanometer Level α-Fe2O3The proterties and performance of material, fully develop α-Fe2O3The various performances and application value of nano material, it is nano level α-Fe2O3Powder prepares the highest attention of researcher.
Scientist successfully have developed and many new prepare nanometer alpha-Fe in recent years2O3The methods and techniques of powder, mainly have Vapor phase method, solid phase method, hydro-thermal method, microwave irradiation, electrochemical synthesis, homogeneous precipitation method, agglutinating nature yeast, conbustion synthesis Method and liquid-phase catalysis phase inversion etc., these method usual conditions control require of a relatively high, long preparation period, especially with Microwave and electrochemical process prepare nano-powder, and process parameter control is very strict, and catalytic phaseinversion method needs to find suitable phase Reforming catalyst etc., these operation requirements cause product cost high, and process is numerous and diverse.And the present invention carries out nano oxygen using urea Change the technology of preparing of iron, not only increase nano-sized iron oxide and prepare approaches and methods, and good product dispersibility, the pattern for preparing Size is controllable and good stability, is a kind of novel magnetic ferric oxide nano powder that easy to operate, process is easily-controllable, product is homogeneous Body material preparation method.
The content of the invention
It is an object of the invention to overcome defect of the prior art, there is provided a kind of new urea disperses source of iron, and decomposes Generation precipitation reaction, α-Fe are prepared through calcining2O3The controllable method for preparing of magnetic nano powder material.Not only low cost, operates letter It is single and low for equipment requirements, environmental protection, product particle is uniform, stable performance, realizes α-Fe2O3Magnetic nano powder material Controllable preparation.
To reach above-mentioned technical purpose, the technical solution adopted by the present invention is as follows:
A kind of α-Fe of the present invention2O3The preparation method of magnetic nano powder material, concrete operations are as follows:
(1)Inorganic metal molysite and urea is soluble in water according to certain mol ratio, stirring to being completely dissolved, using urea and The dispersed effect of water is obtained homogeneous solution;
(2)Solution is heated, is decomposed using urea and Fe3+Precipitation reaction, after reaction terminates, centrifugation obtains solid, and with steaming Distilled water is washed 3-5 times, obtains Fe (OH)3Solid;
(3)Solid is placed in drying box and is dried, it is polished to be placed in temperature programmed control stove, calcined in air ambient, it is natural Room temperature is cooled to, α-Fe are obtained2O3Magnetic nano powder material.
Preferably, step(1)In, inorganic metal molysite is iron chloride or ferric nitrate, and Fe3+Mol ratio with urea is not small In 5:1, Fe3+Concentration 0.5-3.0 mol/L in water.
Preferably, step(2)In, between 85-98 DEG C, the reaction time is 1-6 h to solution warming temperature.
Preferably, step(3)In, the calcining heat is 500-700 DEG C, calcining heat 1-4 h.
Beneficial effects of the present invention are as follows:
The present invention carries out the dispersion of source of iron and decomposes precipitation source of iron using urea, and α-Fe are prepared with reference to calcination2O3Magnetic Nano Powder body material, its method is simple and direct, easy controlled operation, and product is homogeneous, stable performance, is also the system of iron oxide magnetic nano powder body material It is standby to have opened up new method and approach, for urea for the enterprise of byproduct provides new high added value two generations product, and use This method prepares α-Fe2O3Magnetic nano powder material feedstock is abundant, and low cost, process is simple and easy to control, without special device, if It is standby less demanding, the pattern and performance of product can be efficiently controlled by controlling decomposable process and calcining machine system, realize α- Fe2O3Effective controllable preparation of magnetic nano powder material, with practical value very high.
Brief description of the drawings
Fig. 1 is α-Fe prepared by embodiment 12O3The ESEM panorama sketch of magnetic nano powder material;
Fig. 2 is α-Fe prepared by embodiment 12O3The ESEM enlarged drawing of magnetic nano powder material;
Fig. 3 is α-Fe prepared by embodiment 12O3The X diffraction patterns of magnetic nano powder material;
Fig. 4 is α-Fe prepared by embodiment 12O3The hysteresis curve figure of magnetic nano powder material.
Specific embodiment
With reference to specific embodiments and the drawings content, the invention will be further elaborated, so that those skilled in the art It is better understood from technical scheme.
Embodiment 1:α-Fe2O3The preparation of magnetic nano powder material
Compound concentration is the FeCl of 0.8 mol/L3Solution, accurately pipettes 50 mL and is transferred to 250 mL conical flasks, according to urea with Fe3+Mol ratio 10:1 precise urea is added in 250 mL conical flasks, stirring and dissolving, and solution is warming up into 85 DEG C, stirring React 4 h., by precipitation with water washing is distilled 5 times, be placed in precipitation in drying box after centrifugation by centrifugation, after drying Presoma.Presoma is ground, is put into temperature programming resistance furnace and is calcined 4 h at 600 DEG C, natural cooling obtains α-Fe2O3Magnetic Nano-powder material.
Fig. 1 is α-Fe manufactured in the present embodiment2O3The scanning electron microscopic picture panorama sketch of magnetic nano powder material, from panorama Figure can see, and the ferric oxide nano powder material of preparation is in granular form, and diameter is evenly distributed.
Fig. 2 is α-Fe manufactured in the present embodiment2O3The scanning electron microscopic picture enlarged drawing of magnetic nano powder material, from Electronic Speculum Figure is as can be seen that α-Fe2O3The diameter of magnetic nano powder material is about 240 nm.
Fig. 3 be the present embodiment described under the conditions of prepare α-Fe2O3The X-ray diffraction spectrum and α of magnetic nano powder material- Fe2O3Standard PDF cards(JCPDS No. 33-0664)Comparison diagram;It can be seen that the X-ray diffraction peak position of product With α-Fe2O3Standard PDF cards are corresponded to completely, it may be determined that product thing is mutually α-Fe2O3
Fig. 4 be the present embodiment described under the conditions of prepare α-Fe2O3The hysteresis curve figure of magnetic nano powder material;Its magnetic Hysteresis curves show, α-Fe2O3Magnetic nano powder material has typical soft magnetic characteristic, and its saturation magnetization is 0.36 emu/ g。
Embodiment 2:α-Fe2O3The preparation of magnetic nano powder material
Compound concentration is the Fe (NO of 3.0 mol/L3)3Solution, accurately pipettes 50 mL and is transferred to 250 mL conical flasks, according to urine Element and Fe3+Mol ratio 5:1 precise urea is added in 250 mL conical flasks, and solution is warming up to 90 DEG C by stirring and dissolving, is stirred Mix 1 h of reaction., by precipitation with water washing is distilled 5 times, be placed in precipitation in drying box after centrifugation, after drying by centrifugation Obtain presoma.Presoma is ground, is put into temperature programming resistance furnace and is calcined 2 h at 500 DEG C, natural cooling obtains α-Fe2O3Magnetic Property nano-powder material, its saturation magnetization be 0.35 emu/g.
Embodiment 3:α-Fe2O3The preparation of magnetic nano powder material
Compound concentration is the FeCl of 0.5 mol/L3Solution, accurately pipettes 50 mL and is transferred to 250 mL conical flasks, according to urea with Fe3+Mol ratio 8:1 precise urea is added in 250 mL conical flasks, stirring and dissolving, and solution is warming up into 98 DEG C, and stirring is anti- Answer 6 h., by precipitation with water washing is distilled 5 times, be placed in precipitation in drying box after centrifugation by centrifugation, before being obtained after drying Drive body.Presoma is ground, is put into temperature programming resistance furnace and is calcined 3 h at 700 DEG C, natural cooling obtains α-Fe2O3Magnetic is received Rice powder body material, its saturation magnetization is 0.41 emu/g.
Embodiment 4:α-Fe2O3The preparation of magnetic nano powder material
Compound concentration is the FeCl of 1.6 mol/L3Solution, accurately pipettes 50 mL and is transferred to 250 mL conical flasks, according to urea with Fe3+Mol ratio 6:1 precise urea is added in 250 mL conical flasks, stirring and dissolving, and solution is warming up into 85 DEG C, and stirring is anti- Answer 2 h., by precipitation with water washing is distilled 5 times, be placed in precipitation in drying box after centrifugation by centrifugation, before being obtained after drying Drive body.Presoma is ground, is put into temperature programming resistance furnace and is calcined 4 h at 600 DEG C, natural cooling obtains α-Fe2O3Magnetic is received Rice powder body material, its saturation magnetization is 0.34 emu/g.
Embodiment 5:α-Fe2O3The preparation of magnetic nano powder material
Compound concentration is the Fe (NO of 1.0 mol/L3)3Solution, accurately pipettes 50 mL and is transferred to 250 mL conical flasks, according to urine Element and Fe3+Mol ratio 5:1 precise urea is added in 250 mL conical flasks, and solution is warming up to 95 DEG C by stirring and dissolving, is stirred Mix 3 h of reaction., by precipitation with water washing is distilled 5 times, be placed in precipitation in drying box after centrifugation, after drying by centrifugation Obtain presoma.Presoma is ground, is put into temperature programming resistance furnace and is calcined 4 h at 700 DEG C, natural cooling obtains α-Fe2O3Magnetic Property nano-powder material, its saturation magnetization be 0.40 emu/g.

Claims (6)

1. a kind of α-Fe2O3Magnetic nano powder material, it is characterised in that the material is in granular form, and diameter is evenly distributed;Directly Footpath is about 240 nm.
2. a kind of α-Fe2O3The preparation method of magnetic nano powder material, it is characterised in that carry out in accordance with the following steps:
(1)Inorganic metal molysite and urea is soluble in water according to certain mol ratio, stirring to being completely dissolved, using urea and The dispersed effect of water is obtained homogeneous solution;
(2)Solution is heated, is decomposed using urea and Fe3+Precipitation reaction, after reaction terminates, centrifugation obtains solid, and with steaming Distilled water is washed 3-5 times, obtains precipitation solid;
(3)Solid is placed in drying box and is dried, it is polished to be placed in temperature programmed control stove, calcined in air ambient, it is natural Room temperature is cooled to, α-Fe are obtained2O3Magnetic nano powder material.
3. a kind of α-Fe according to claim 22O3The preparation method of magnetic nano powder material, it is characterised in that step (1)Described in inorganic metal molysite be iron chloride or ferric nitrate.
4. a kind of α-Fe according to claim 22O3The preparation method of magnetic nano powder material, it is characterised in that step (1)Described in Fe3+Mol ratio with urea is not less than 5:1, and Fe3+Concentration is 0.5-3.0 mol/L.
5. a kind of α-Fe according to claim 22O3The preparation method of magnetic nano powder material, it is characterised in that step Suddenly(2)Described in solution warming temperature between 85-98 DEG C, the reaction time be 1-6 h.
6. a kind of α-Fe according to claim 22O3The preparation method of magnetic nano powder material, it is characterised in that step Suddenly(3)Described in calcining heat be 500-700 DEG C, calcining heat 1-4 h.
CN201611131662.8A 2016-12-09 2016-12-09 A kind of α Fe2O3The preparation method of magnetic nano powder material Pending CN106745305A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108371938A (en) * 2018-05-09 2018-08-07 上海大学 Mesoporous magnetic Nano iron oxide material, preparation method and applications
CN108502932A (en) * 2018-06-06 2018-09-07 江苏大学 A kind of FeOOH microns of octahedral preparation method
CN108682847A (en) * 2018-05-07 2018-10-19 苏州大学 A kind of more shell hollow microsphere shape α-Fe2O3Material, preparation method and applications
CN108855085A (en) * 2018-07-25 2018-11-23 黑龙江省科学院自然与生态研究所 A kind of preparation method of high surface defect iron oxide water process ozone catalyst
CN110615482A (en) * 2019-10-08 2019-12-27 吉林大学 Method for preparing epsilon-phase iron oxide by ball milling method
WO2020006977A1 (en) * 2018-07-04 2020-01-09 中国科学院南京土壤研究所 Metal-organic framework material fertilizer and preparation method therefor

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CN105110381A (en) * 2015-09-15 2015-12-02 昆明理工大学 Method for preparing nanopore alpha-Fe2O3

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CN105110381A (en) * 2015-09-15 2015-12-02 昆明理工大学 Method for preparing nanopore alpha-Fe2O3

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刘树信等: "均匀沉淀法制备α-Fe2O3超细粉体的研究", 《人工晶体学报》 *
张杰等: "纳米α-Fe2O3粒子的湿法制备", 《辽宁化工》 *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108682847A (en) * 2018-05-07 2018-10-19 苏州大学 A kind of more shell hollow microsphere shape α-Fe2O3Material, preparation method and applications
CN108682847B (en) * 2018-05-07 2021-03-16 苏州大学 Multi-shell hollow microspherical alpha-Fe2O3Material, preparation method and application thereof
CN108371938A (en) * 2018-05-09 2018-08-07 上海大学 Mesoporous magnetic Nano iron oxide material, preparation method and applications
CN108502932A (en) * 2018-06-06 2018-09-07 江苏大学 A kind of FeOOH microns of octahedral preparation method
WO2020006977A1 (en) * 2018-07-04 2020-01-09 中国科学院南京土壤研究所 Metal-organic framework material fertilizer and preparation method therefor
CN108855085A (en) * 2018-07-25 2018-11-23 黑龙江省科学院自然与生态研究所 A kind of preparation method of high surface defect iron oxide water process ozone catalyst
CN108855085B (en) * 2018-07-25 2021-03-16 黑龙江省科学院自然与生态研究所 Preparation method of ozone catalyst for treating iron oxide water with high surface defects
CN110615482A (en) * 2019-10-08 2019-12-27 吉林大学 Method for preparing epsilon-phase iron oxide by ball milling method
CN110615482B (en) * 2019-10-08 2021-09-24 吉林大学 Method for preparing epsilon-phase iron oxide by ball milling method

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