CN101497463B - Method for preparing gamma-Fe2O3 nanoparticle by two-step precipitation - Google Patents
Method for preparing gamma-Fe2O3 nanoparticle by two-step precipitation Download PDFInfo
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- CN101497463B CN101497463B CN2009101033336A CN200910103333A CN101497463B CN 101497463 B CN101497463 B CN 101497463B CN 2009101033336 A CN2009101033336 A CN 2009101033336A CN 200910103333 A CN200910103333 A CN 200910103333A CN 101497463 B CN101497463 B CN 101497463B
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Abstract
The invention provides a method for preparing gamma-Fe2O3 nanoparticles by a two-step precipitation method, which comprises the following steps: 1, a coprecipitation method is adopted to prepare an FeOOH/Mg(OH)2 precursor; and 2, a hydroxide precursor is subjected to heat treatment in an FeCl2 solution, and the obtained product is cooled to a room temperature and then is precipitated again to produce the gamma-Fe2O3 nanoparticles. A geometric median particle diameter of the gamma-Fe2O3 nanoparticles is around 8nm, and a specific saturation magnetization is higher than 70emu/g. The method has the advantages of unique formation mechanism, low cost of raw materials, and easy operation of the preparation process; and the prepared gamma-Fe2O3 nanoparticles are mainly spherical, and have small particle diameters and high saturation magnetization.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to ferromagnetic γ-Fe
2O
3The preparation of nanoparticle.
Background technology
Particle diameter is that the magnetic nanometer particles of 1～100nm scope is important nano material, wherein γ-Fe
2O
3Magnetic nanometer particles is because chemical property is stable, magnetic is strong and be used for biomedicine field (as the separation of mark magnetic carrier, biochemical product, nuclear magnetic resonance contrast-enhancing agent etc.) and other technical field, as high-density magnetic memory device, magnetic cooling system and magnetic liquid.γ-Fe
2O
3The technology of preparing of nanoparticle has coprecipitation method, microemulsion method, thermal decomposition method, hydrothermal method and evaporation-condensation method etc.Wherein coprecipitation method be use the most general method, this legal system is equipped with γ-Fe
2O
3Its specific saturation magnetization of nanoparticle is about 50emu/g, and how much median particle diameters are about 10nm.
Summary of the invention
The present invention proposes the two-step precipitation legal system and be equipped with γ-Fe
2O
3The method of nanoparticle.This method has unique formation mechanism, and material cost is low, the preparation process easy handling.Prepared γ-Fe
2O
3Nanoparticle is spherical substantially, and particle diameter is little, the saturation magnetization height.
Preparation method of the present invention is specific as follows:
The first step precipitation: presoma preparation
In alkaline medium, co-precipitation Fe
3+-Mg
2+The mixture of the aqueous solution is to obtain oxyhydroxide presoma throw out.
(1) FeCl of preparation 2-4M concentration
3Mg (the NO of the aqueous solution (solution 1), 1-3M concentration
3)
2(solution 2 is by every liter of Mg (NO for the aqueous solution
3)
2The ratio of 5 moles of HCl of solution adds HCl).Prepare the NaOH aqueous solution (solution 3) of 0.7M concentration in addition
(2) be to choose an amount of solution 1 and solution 2 at 1～3: 1 according to Fe, Mg mol ratio, with solution 1 pour into obtain in the solution 2 solution 2 '.Be to choose an amount of solution 3 at 1: 10 according to solution 2 ' again with the volume ratio of solution 3.Under agitation solution 2 ' pour into is fast obtained in the solution 3 solution 3 '.
(3) heated solution 3 ' extremely boiling under agitation.Keep boiling 1 minute, stop heating then, naturally cool to room temperature.After 1 hour, precipitation of hydroxide is come out.
(4) outwell clear liquid, stay throw out.Use HNO
3The aqueous solution repeatedly cleans, to pH=7～8.
The second step precipitation: produce γ-Fe
2O
3Particulate
(1) FeCl of preparation 0.1-0.5M concentration
2The aqueous solution (solution 4)
(2) oxyhydroxide that the first step precipitation is obtained is poured in the solution 4, gets solution 5, and the volume ratio of throw out and solution 4 is 1: 10;
(3) under agitation heated solution 5 to boiling.Keep boiling 5～60 minutes, stop heating then, be cooled to room temperature.
After 1 hour, new throw out-γ-Fe
2O
3Particulate produces.
(4) clean with distilled water.
(5) with acetone dehydration, drying, make γ-Fe
2O
3Nanoparticle.
Prepared γ-Fe
2O
3The particle diameter of nanoparticle is at 3-18nm, and specific saturation magnetization is higher than 70emu/g.
Present method material cost is low, the preparation process easy handling, prepared γ-Fe
2O
3Nanoparticle is spherical substantially, and particle diameter is little, the saturation magnetization height.
Description of drawings
Fig. 1 is that this law prepares γ-Fe
2O
3The transmission electron microscope image of particulate
Fig. 2 is the γ-Fe of this law preparation
2O
3The magnetzation curve of nanoparticle
Embodiment one:
One, precipitate for the first time: coprecipitation method prepares presoma
1. the preparation of solution
(1) solution 1.: FeCl
3The aqueous solution (40ml, 1mol/L)
(2) solution 2.: Mg (NO
3)
2(10ml, 2mol/L), other adds the HCl of 0.05mol to the aqueous solution
(3) solution is 3.: and the NaOH aqueous solution (500ml, 0.7mol/L)
2. mix
(1) solution 1. pour into solution obtain in 2. solution 2. '
(2) solution 3. pour into solution 2. ' obtain solution 3. '
3. reaction
(1) with solution 3. ' on electric furnace, be heated to boiling, do not stop in the heat-processed to stir.
(2) boiling was taken off from process furnace after 5 minutes, naturally cooling, and the reddish-brown precipitation that engenders in the process of cooling, postprecipitation finished in about 2 hours.
4. clean
(1) scavenging solution preparation
0.01mol/L HNO
3The aqueous solution
(2) clean
In throw out and scavenging solution volume ratio is that 1: 5 ratio is mixed, and fully stirs ((1～1.2) * 10 of centrifugation then
3Rev/min).After outwelling upper clear supernate, add scavenging solution more equally and clean.Repeated multiple times is until PH～7-8.
Two, precipitate for the second time: FeCl
2Processing of Preparation γ-Fe
2O
3Nanoparticle
1. solution preparation
Solution is 4.: FeCl
2The aqueous solution (400ml, 0.25mol/L)
2. mix
4. the throw out that obtains in the settling step first time is mixed with solution, obtain solution 5.
3. reaction
(1) 5. solution is heated to boiling on electric furnace, keeps boiling 30 minutes.Keep uninterrupted the stirring therebetween.
(2) take off naturally cooling from electric furnace.Engender black precipitate in the process of cooling.
4. clean
Clean three times with distilled water
5. dry
(1) be that sedimentary 4～5 times acetone mixes with volume, centrifugation is dewatered then, and this step repeats 2～3 times.
(2) dewatered product is changed in the moisture eliminator.Can obtain anhydrous exsiccant γ-Fe after 24 hours
2O
3Particulate
Embodiment two:
One, precipitate for the first time: coprecipitation method prepares presoma
Identical with embodiment one.
Two, precipitate for the second time: FeCl
2Processing of Preparation γ-Fe
2O
3Nanoparticle
1. solution preparation
Solution is 4.: FeCl
2The aqueous solution (400ml, 0.5mol/L)
2-5 is identical with embodiment one.
Embodiment three:
One, precipitate for the first time: coprecipitation method prepares presoma
Identical with embodiment one.
Two, precipitate for the second time: FeCl
2Processing of Preparation γ-Fe
2O
3Nanoparticle
1-2 is identical with embodiment one.
3. reaction
(1) 5. solution is heated to boiling on electric furnace, keeps boiling 45 minutes.Keep uninterrupted the stirring therebetween.
(2) take off naturally cooling from electric furnace.Engender black precipitate in the process of cooling.
4-5 is identical with embodiment one.
The form of particulate and particle diameter
The form that obtains particulate with transmission electron microscope is spherical substantially, as shown in Figure 1.By analysis, diameter of particle is lognormal distribution, how much median particle diameter d
gBe 7.9nm, distribution bias ln σ
gBe 0.29.
The specific magnetising moment of particulate
Carry out the measurement of the specific magnetising moment with vibrating sample magnetometer, obtained the magnetzation curve of specific magnetization σ and magnetic field H relation, as shown in Figure 2, by analysis, its specific saturation magnetization σ
sBe 75emu/g.
Claims (2)
1. the two-step precipitation legal system is equipped with γ-Fe
2O
3The method of nanoparticle comprises following two steps:
The first step: presoma preparation
In alkaline medium, co-precipitation Fe
3+-Mg
2+The mixture of the aqueous solution, to obtain oxyhydroxide presoma throw out:
(1) FeCl of preparation 2-4M concentration
3The aqueous solution, ie in solution 1; Mg (the NO of preparation 1-3M concentration
3)
2The aqueous solution is by every liter of Mg (NO
3)
2The ratio of 5 moles of HCl of solution adds HCl, ie in solution 2; Prepare the NaOH aqueous solution of 0.7M concentration in addition, ie in solution 3;
(2) be to choose solution 1 and solution 2 at 1～3: 1 according to Fe, Mg mol ratio, with solution 1 pour into obtain in the solution 2 solution 2 '; Be to choose solution 3 at 1: 10 according to solution 2 ' again with the volume ratio of solution 3, under agitation solution 2 ' pour into is fast obtained in the solution 3 solution 3 ';
(3) under agitation heated solution 3 ' to boiling, maintenance boiling 1 minute stops heating then, naturally cools to room temperature, and after 1 hour, precipitation of hydroxide is come out;
(4) outwell clear liquid, stay throw out, use HNO
3The aqueous solution repeatedly cleans, to pH=7～8;
Second step: γ-Fe
2O
3Nanoparticle forms
(1) FeCl of preparation 0.1-0.5M concentration
2The aqueous solution, ie in solution 4;
(2) oxyhydroxide that the first step precipitation is obtained is poured in the solution 4, gets solution 5; The volume ratio of throw out and solution 4 is 1: 10;
(3) under agitation heated solution 5 keeps boiling 5～60 minutes to boiling, stops heating then, is cooled to room temperature, after 1 hour, and throw out-γ-Fe
2O
3Particulate produces;
(4) throw out that (3) are obtained cleans with distilled water, with acetone dehydration, drying, makes γ-Fe again
2O
3Nanoparticle.
2. two-step precipitation legal system according to claim 1 is equipped with γ-Fe
2O
3The method of nanoparticle is characterized in that prepared γ-Fe
2O
3The particle diameter of nanoparticle is at 3-18nm, and specific saturation magnetization is higher than 70emu/g.
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|---|---|---|---|
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|---|---|---|---|
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| CN101497463B true CN101497463B (en) | 2011-04-13 |
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|---|---|---|---|---|
| CN102285692B (en) * | 2011-06-16 | 2013-03-27 | 西南大学 | Preparation of colloid with strong magneto optic effect |
| CN102910682B (en) * | 2012-09-29 | 2014-08-27 | 西南大学 | Preparation method of gamma-Fe2O3/ZnFe2O4 magnetic composite nano particle |
| CN103112902B (en) * | 2013-03-12 | 2014-12-03 | 西南大学 | Method for preparing composite nanoparticles with adjustable magnetism |
| CN103466716B (en) * | 2013-06-09 | 2016-03-23 | 西南大学 | A kind of preparation method of magnetic Nano crystallite of adjustable form |
| CN106311268A (en) * | 2015-07-06 | 2017-01-11 | 中国石油化工股份有限公司 | Method for improving performance of methanol synthesis catalyst |
| CN105086557B (en) * | 2015-09-28 | 2017-11-07 | 沈阳建筑大学 | Doped ferric oxide powder for anti-corrosive paint of epoxy resin and preparation method 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 |
| CN110252304B (en) * | 2018-03-12 | 2021-12-17 | 中国石油化工股份有限公司 | Iron-based catalyst, preparation method and application thereof, carbon nano tube and preparation method thereof |
| CN110694591A (en) * | 2019-09-05 | 2020-01-17 | 武汉东湖科创中试基地科技有限公司 | Preparation method and application of Fe-GO/Cs composite microspheres |
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