CN101100314A - Method for preparing gamma-Fe2O3 nano magnetic material - Google Patents

Method for preparing gamma-Fe2O3 nano magnetic material Download PDF

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Publication number
CN101100314A
CN101100314A CNA200710041853XA CN200710041853A CN101100314A CN 101100314 A CN101100314 A CN 101100314A CN A200710041853X A CNA200710041853X A CN A200710041853XA CN 200710041853 A CN200710041853 A CN 200710041853A CN 101100314 A CN101100314 A CN 101100314A
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China
Prior art keywords
magnetic material
urea
ammonium oxalate
iron nitrate
aqueous solution
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CNA200710041853XA
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CN100522823C (en
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李春忠
王素芬
顾锋
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East China University of Science and Technology
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East China University of Science and Technology
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Abstract

This invention discloses a method for preparing gamma-Fe203 nanometer magnetic material. The procedures are: ferrous nitrate and urea, ammonium oxalate solution are heated under 130-170deg.C for 4-9hrs, and then fed in a preheated environment of 300-600deg.C for 10-30minites, so obtaining this inventive gammer-fe203 nanometer powder. This invention has advantages of: simple process, safety, no need of protective atmosphere, short reaction time (10-30 minites), energy-saving, low cost of raw material, high yield, high pureness, definitive constituents and crystal-form, excellent magnetic property.

Description

A kind of γ-Fe for preparing 2O 3The method of nano magnetic material
Technical field
The present invention relates to a kind of γ of preparation-Fe 2O 3The method of nano magnetic material.
Background technology
γ-Fe 2O 3It is very widely functional material of a kind of application.Owing to have good magnetic, catalysis and air-sensitive performance and absorption and the shielding effect good to ultraviolet ray, it is used as magnetic recording material, magnetic liquid, electromagnetic wave absorbent material, gas sensor, catalyzer, nonlinear optical material, all has a good application prospect in fields such as electronics, petrochemical complex, environmental protection and biological medicine engineerings.
Present γ-Fe 2O 3Preparation become the focus of people research.Preparation γ-Fe 2O 3The most frequently used method of nano powder is liquid-phase precipitation method, obtains γ-Fe through steps such as precipitating, dewater, reduce, reoxidize 2O 3This method complex process yields poorly, and the quality of products obtained therefrom is still waiting to improve.
Recently the preparation method of development also has sol-gel method, laser vapor phase method, pyrolysis method, microemulsion method, high-energy ball milling method, sputtering method, vapour deposition process, solid phase method etc.These methods have exists complicated operation, process to be difficult to control, quality product is difficult to guarantee, what have exists weak points such as facility investment is big, processing condition are harsh, productive rate is lower, be difficult to apply.
Preparation γ-the Fe that therefore explore that a kind of simple to operate, process is easy to control, output height, product quality can be guaranteed and have certain prospects for commercial application 2O 3Method, be the target that researcher is pursued.
Summary of the invention
The objective of the invention is to propose a kind of γ of preparation-Fe 2O 3The method of nano magnetic material to overcome existing preparation method's deficiency, satisfies the needs of practical application.
Method of the present invention comprises the steps:
With the aqueous solution of ferric nitrate, urea and ammonium oxalate, at 130~170 ℃, preferred 150 ℃ of lower heating 4-9h place the environment that is warming up in advance 300-600 ℃ to react then 10-30 minute, can obtain γ-Fe 2O 3Nano powder;
In the said aqueous solution, the molar weight of urea is 3-8 a times of iron nitrate mole, and the molar weight of said ammonium oxalate is 3-6 a times of iron nitrate mole, and in the aqueous solution, the content of iron nitrate is 1.00~1.35g/ml;
The product that adopts above-mentioned steps to obtain, more loose, by the pattern of transmission electron microscope and scanning electron microscopic observation product, laminar structured for the nano particle Adhesion formation, the average grain diameter of particle is 30-40nm, the crystalline phase of product consists of γ-Fe 2O 3(JCPDS No.39-1364), saturation magnetization is 45~55emu/g.
The present invention adopts firing method to synthesize fast γ-Fe 2O 3Nano powder; this method technology simple, safe and reliable (air atmosphere need not special atmosphere protection), reaction time short (10-30 minute), energy savings, raw material are cheap, product output height and products therefrom purity height, component and crystal formation are determined, magnetic property is good.
Description of drawings
Fig. 1 obtains the x-ray diffraction pattern of product for embodiment 1.
Embodiment
Embodiment 1
Take by weighing the 8.08g iron nitrate, 4.0g urea, the 10.0g ammonium oxalate adds the 7.0ml deionized water.Put into baking oven after fully stirring 30min, obtain the mixture of thickness at 150 ℃ of lower baking 5h.
Said mixture is poured in the crucible, put into the retort furnace that is warmed up to 400 ℃ in advance and reacted 15 minutes, can obtain final product.Product is the laminar structured of nano particle composition, and crystallinity is good, and saturation magnetization is 49emu/g.The crystalline phase of product is formed as shown in Figure 1.
Embodiment 2
Take by weighing the 8.08g iron nitrate, 5.0g urea, the 15.0g ammonium oxalate adds the 8.0ml deionized water.Put into baking oven after fully stirring 30min, obtain the mixture of thickness at 130 ℃ of lower baking 7h.Said mixture is poured in the crucible, put into the retort furnace that is warmed up to 500 ℃ in advance and reacted 10 minutes, can obtain final product.Product is the laminar structured of nano particle composition, and crystallinity is good, and saturation magnetization is 48emu/g.
Embodiment 3
Take by weighing the 8.08g iron nitrate, 7.0g urea, the 16.0g ammonium oxalate adds the 11.0ml deionized water.Put into baking oven after fully stirring 30min, obtain the mixture of thickness at 170 ℃ of lower baking 5h.Said mixture is poured in the crucible, put into the retort furnace that is warmed up to 400 ℃ in advance and reacted 25 minutes, can obtain final product.Product is the laminar structured of nano particle composition, and crystallinity is good, and saturation magnetization is 50emu/g.
Embodiment 4
Take by weighing the 8.08g iron nitrate, 4.5g urea, the 13.5g ammonium oxalate adds the 8.0ml deionized water.Put into baking oven after fully stirring 30min, obtain the mixture of thickness at 150 ℃ of lower baking 6h.Said mixture is poured in the crucible, put into the retort furnace that is warmed up to 600 ℃ in advance and reacted 10 minutes, can obtain final product.Product is the laminar structured of nano particle composition, and crystallinity is good, and saturation magnetization is 45emu/g.

Claims (4)

1. one kind prepares γ-Fe 2O 3The method of nano magnetic material is characterized in that, comprises the steps: the aqueous solution with ferric nitrate, urea and ammonium oxalate, at 130~170 ℃ of lower heating 4-9h, places then the environment that is warming up in advance 300-600 ℃ to react 10-30 minute, can obtain γ-Fe 2O 3Nano powder.
2. method according to claim 1 is characterized in that, heats 4-9h down at 150 ℃.
3. method according to claim 1 is characterized in that, in the said aqueous solution, the molar weight of urea is 3-8 a times of iron nitrate mole, the molar weight of said ammonium oxalate is 3-6 a times of iron nitrate mole, and in the aqueous solution, the content of iron nitrate is 1.00~1.35g/ml.
4. according to claim 1,2 or 3 described methods, it is characterized in that the crystalline phase of product consists of γ-Fe 2O 3(JCPDS No.39-1364), saturation magnetization is 45~55emu/g.
CNB200710041853XA 2007-06-11 2007-06-11 Method for preparing gamma-Fe2O3 nano magnetic material Expired - Fee Related CN100522823C (en)

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Application Number Priority Date Filing Date Title
CNB200710041853XA CN100522823C (en) 2007-06-11 2007-06-11 Method for preparing gamma-Fe2O3 nano magnetic material

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CN100522823C CN100522823C (en) 2009-08-05

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103149354A (en) * 2013-01-29 2013-06-12 南昌大学 Fast detecting method for food-borne pathogenic bacteria based on gamma-Fe2O3 mano-material immune magnetic separation
CN105948132A (en) * 2016-05-06 2016-09-21 上海应用技术学院 Preparation method of three-dimensional gamma-Fe2O3 nano material and application thereof
CN106430331A (en) * 2016-09-19 2017-02-22 青岛鼎元磁材有限公司 Preparation method of high-coercivity, high-remanence and anti-fake magnetic powder
CN108807882A (en) * 2018-05-24 2018-11-13 江西师范大学 A kind of Fe with porous octahedral structure2O3/Fe3O4The preparation method of@C/G composite materials

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103149354A (en) * 2013-01-29 2013-06-12 南昌大学 Fast detecting method for food-borne pathogenic bacteria based on gamma-Fe2O3 mano-material immune magnetic separation
CN105948132A (en) * 2016-05-06 2016-09-21 上海应用技术学院 Preparation method of three-dimensional gamma-Fe2O3 nano material and application thereof
CN105948132B (en) * 2016-05-06 2017-05-17 上海应用技术学院 Preparation method of three-dimensional gamma-Fe2O3 nano material and application thereof
CN106430331A (en) * 2016-09-19 2017-02-22 青岛鼎元磁材有限公司 Preparation method of high-coercivity, high-remanence and anti-fake magnetic powder
CN108807882A (en) * 2018-05-24 2018-11-13 江西师范大学 A kind of Fe with porous octahedral structure2O3/Fe3O4The preparation method of@C/G composite materials
CN108807882B (en) * 2018-05-24 2022-04-26 江西师范大学 Fe with porous octahedral structure2O3/Fe3O4Preparation method of @ C/G composite material

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