CN103112902A - Method for preparing composite nanoparticles with adjustable magnetism - Google Patents
Method for preparing composite nanoparticles with adjustable magnetism Download PDFInfo
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- CN103112902A CN103112902A CN2013100784599A CN201310078459A CN103112902A CN 103112902 A CN103112902 A CN 103112902A CN 2013100784599 A CN2013100784599 A CN 2013100784599A CN 201310078459 A CN201310078459 A CN 201310078459A CN 103112902 A CN103112902 A CN 103112902A
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- aqueous solution
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Abstract
The invention discloses a method for preparing composite nanoparticles with adjustable magnetism. The method comprises the following steps: the precursor preparing step comprises the substeps of coprecipitating a mixture of Fe<3+> and Mg<2+> aqueous solutions in an alkaline medium, and thus obtaining a hydroxide precursor; and 2 the composite nanoparticle synthesizing step comprises the substeps of (1) chemically inducing the precursor in a FeCl2 solution to generate phase change, and thus generating a Fe2O3 nanocrystal; and (2) adding ZnCl2 and NaOH solutions, generating regulation reaction on a Fe2O3 nanocrystal surface, forming a ZnFe2O4 layer on a Fe2O3 nanocrystal epitaxy, and forming an outermost Zn(OH)2 layer on the ZnFe2O4 layer so as to obtain the composite nanoparticle. The method is low in raw material cost, moderate in technological condition and easy to operate in a preparation process; and the prepared magnetic composite nanoparticles are multilayer Fe2O3/ZnFe2O4 composite nanoparticles wrapped by Zn(OH)2, the magnetism of the composite nanoparticles is distributed in a graded manner from inside to outside, and the composite nanoparticle is small in size and has good dispersibility.
Description
Technical field
The invention belongs to field of nanometer material technology, be specifically related at-Fe
2O
3During the Zn of nanoparticle modulation was synthetic, the alkaline condition by controlling solution was with the method for the different composite nano particle of the preparation specific magnetising moment.
Background technology
Nanoparticle be three dimension scale all less than the nano material of 100nm, in inorganic or organic materials, many physical phenomenons have 1 to 100nm characteristic length scale.Magnetic nanometer particles is important functional materials, and important value is arranged in fundamental research and applied research.For example, magnetic nanometer particles is scattered in the magnetic liquid that forms in silicone oil and can be used as a kind of good sealing material.
Composite nano materials is at least one mutually for two-phase or multiphase material of nanoscale.The combination of different physics or chemical property causes matrix material may have strange character fully.Composite nano particle is generally inclusion.The composite nano particle with gradient magnetic that is made of strong magnetic (ferromagnetic or Ferrimagnetic) core and weak magnetic (antiferromagnetic or paramagnetic) shell may have dispersed preferably.One of important channel of preparation nucleocapsid structure composite nano particle is to carry out surface modulation in the body material building-up process of heart core section, thereby forms heterogeneous upper layer.G-Fe
2O
3Belong to the ferrimagnetism material, ZnFe
2O
4Belong to antiferromagnetic substance, Zn (OH)
2Belong to paramagnetic substance.The g-Fe for preparing the different specific magnetising moment by controlling synthesis condition
2O
3/ ZnFe
2O
4/ Zn (OH)
2The synthetic method of composite nano particle yet there are no report.
Summary of the invention
The present invention proposes the preparation method of the composite nano particle that a kind of raw materials cost is low, processing condition are gentle, the magnetic of preparation process easy handling is adjustable.
Technical solution of the present invention is as follows:
The preparation method of the composite nano particle that a kind of magnetic is adjustable,
The first step: presoma preparation
In alkaline medium, co-precipitation Fe
3+-Mg
2+The mixture of the aqueous solution obtains the oxyhydroxide presoma;
Second step: composite nano particle synthetic
(1) with presoma at FeCl
2The chemical induction phase transformation occurs in solution, generates g-Fe
2O
3Nanocrystal;
(2) add again ZnCl
2With NaOH solution, make its g-Fe
2O
3The nanocrystal surface produces the modulation reaction, at g-Fe
2O
3The crystal grain extension generates ZnFe
2O
4Layer, and at ZnFe
2O
4Form again Zn (OH) on layer
2Outermost layer, obtain composite nano particle;
The nanoparticle of prepared acquisition is the multilayered structure that different magnetic substances consist of, and the dispersiveness of this kind magnetic nanometer particles better.
Wherein the concrete grammar of the presoma of the first step preparation is as follows:
(1) FeCl of preparation 0.5-4M concentration
3Mg (the NO of the aqueous solution (solution 1), 1-3M concentration
3)
2The aqueous solution (solution 2).According to every liter of Mg (NO
3)
2The aqueous solution adds the ratio of 3-10molHCl to add HCl in Mg (NO
3)
2In solution.Prepare in addition the NaOH aqueous solution (solution 3) of 0.1-2M concentration.
(2) measure appropriate solution 1 and solution 2 according to Fe, Mgmol ratio for 1-3:1; Solution 1 is poured into obtained solution 2' in solution 2.Volume ratio according to solution 2' and solution 3 is that 1:10 chooses appropriate solution 3 again.Under agitation condition, solution 3 is poured into fast and obtained solution 3' in solution 2'.
(3) under agitation heat 3' to boiling.Keep boiling 1-8 minute, then stopped heating, naturally cool to room temperature, and along with temperature descends, presoma is Precipitation gradually.After two hours, precipitin reaction finishes.
(4) clear liquid is outwelled in centrifugation, obtains presoma.
The concrete grammar of the composite nano particle preparation of second step is as follows:
At first prepare the FeCl of 0.1-4M
2The aqueous solution (solution 4), the ZnCl of 0.2-6M
2The aqueous solution (solution 5), the NaOH aqueous solution of 0.1-7M (solution 6).Can be divided into g-Fe by the precursor synthesis composite nano particle
2O
3Nanocrystalline particulate forms and two processes of surface modulation:
A, g-Fe
2O
3Synthesizing of nanoparticle
(1) presoma that the first step precipitin reaction is obtained is poured in solution 4, gets solution 4';
(2) solution 4' under agitation is heated to boiling, and keeps boiling 5-30 minute.
B, surface modulation
(1) add successively ZnCl
2Solution and NaOH solution
(2) continue boiling 5-30 minute, then naturally cool to room temperature.2 hours postprecipitation end of processing.
C, cleaning, drying
(1) take acetone as scavenging solution.The add-on of acetone is 4-6 times of precipitation volume.Centrifugation after fully stirring.This step repeats 3-5 time.
(2) product after cleaning changes in vacuum drying oven.Obtain anhydrous composite magnetic nanoparticle after 24 hours.
Present method raw materials cost is low, processing condition are gentle, the preparation process easy handling, and prepared Magnetic nano composite particles is by Zn (OH)
2The g-Fe of parcel
2O
3/ ZnFe
2O
4The MULTILAYER COMPOSITE nanoparticle, its magnetic is distribution gradient from inside to outside, and this kind nanoparticle size is little, good dispersity.
Description of drawings
Fig. 1 is the magnetzation curve of the composite nano particle of this law embodiment 1 preparation.
Fig. 2 is the transmission electron microscope picture of the composite nano particle of this law embodiment 1 preparation.
Fig. 3 is the magnetzation curve of the composite nano particle of this law embodiment 2 preparations.
Fig. 4 is the transmission electron microscope picture of the composite nano particle of this law embodiment 2 preparations.
Fig. 5 is the magnetzation curve of the composite nano particle of this law embodiment 3 preparations.
Fig. 6 is the transmission electron microscope picture of the composite nano particle of this law embodiment 3 preparations.
Embodiment
Embodiment 1
One, presoma preparation
(1) preparation FeCl
3The aqueous solution (1M, 40mL), ie in solution 1; Preparation Mg (NO
3)
2The aqueous solution (2M, 10mL) adds the HCl of 0.05mol, ie in solution 2; The preparation NaOH aqueous solution (0.7M, 500mL), ie in solution 3.
(2) solution 1 is mixed with solution 2, obtain solution 2'.Under agitation condition, solution 3 is poured in solution 2' fast, obtained solution 3'.
(3) under agitation extremely boiling of heated solution 3'.Keep boiling 5 minutes, then stopped heating.
(4) naturally cool to room temperature.The about complete Precipitation of presoma after two hours.
Two, composite nano particle preparation
(1) preparation FeCl
2The aqueous solution (0.25M, 400mL), ie in solution 4; ZnCl
2The aqueous solution (1M, 50mL), ie in solution 5; The NaOH aqueous solution (0.7M, 5mL), ie in solution 6.
(2) presoma that the first step is synthetic is poured solution 4 into, obtains solution 4';
(3) solution 4' is heated to boiling, and keeps boiling 20 minutes.
(4) add solution 5, then add solution 6.
(5) continue boiling 10 minutes.Stopped heating is cooled to room temperature.The postprecipitation process finished fully in 2 hours.
Three, cleaning, drying
(1) outwell upper clear supernate after Precipitation, the acetone that is 5 times of throw outs with volume mixes with it.Carry out centrifugation, this step repetition 3 times after fully stirring.
(2) precipitation after cleaning changes in vacuum drier, obtains dry anhydrous composite nano particle after 24 hours.
The ratio magnetzation curve of the nanoparticle that embodiment 1 is synthetic as shown in Figure 1, its form is as shown in Figure 2.
Embodiment 2
One, presoma preparation
(1) preparation FeCl
3The aqueous solution (1M, 40mL), ie in solution 1; Preparation Mg (NO
3)
2The aqueous solution (2M, 10mL) adds the HCl of 0.05mol, ie in solution 2; The preparation NaOH aqueous solution (0.7M, 500mL), ie in solution 3.(2) solution 1 is mixed with solution 2, obtain solution 2'.Under agitation condition, solution 3 is poured in solution 2' fast, obtained solution 3'.
(3) under agitation extremely boiling of heated solution 3'.Keep boiling 5 minutes, then stopped heating.
(4) naturally cool to room temperature.The about complete Precipitation of presoma after two hours.
Two, composite nano particle preparation
(1) preparation FeCl
2The aqueous solution (0.25M, 400mL), ie in solution 4; ZnCl
2The aqueous solution (1M, 50mL), ie in solution 5; The NaOH aqueous solution (0.7M, 20mL), ie in solution 6.
(2) presoma that the first step is synthetic is poured solution 4 into, obtains solution 4';
(3) solution 4' is heated to boiling, and keeps boiling 20 minutes.
(4) add solution 5, then add solution 6.
(5) continue boiling 10 minutes.Stopped heating is cooled to room temperature.The postprecipitation process finished fully in 2 hours.
Three, cleaning, drying
With embodiment 1 same operation.
The ratio magnetzation curve of the nanoparticle that embodiment 2 is synthetic as shown in Figure 3, its form is as shown in Figure 4.
Embodiment 3
One, presoma preparation
With embodiment 1 same operation.
Two, composite nano particle preparation
(1) preparation FeCl
2The aqueous solution (0.25M, 400mL), ie in solution 4; ZnCl
2The aqueous solution (1M, 50mL), ie in solution 5; The NaOH aqueous solution (2.1M, 20mL), ie in solution 6.
(2) presoma that the first step is synthetic is poured solution 4 into, obtains solution 4';
(3) solution 4' is heated to boiling, and keeps boiling 20 minutes.
(4) add solution 5, then add solution 6.
(5) continue boiling 10 minutes.Stopped heating is cooled to room temperature.The postprecipitation process finished fully in 2 hours.
Three, cleaning, drying
With embodiment 1 same operation.
The ratio magnetzation curve of the nanoparticle that embodiment 3 is synthetic as shown in Figure 5, its form is as shown in Figure 6.
Claims (4)
1. the composite nano particle preparation method of Adjustable magnetic, comprise the steps:
The first step: presoma preparation
In alkaline medium, co-precipitation Fe
3+-Mg
2+The mixture of the aqueous solution obtains the oxyhydroxide presoma;
Second step: composite nano particle synthetic
(1) with presoma at FeCl
2The chemical induction phase transformation occurs in solution, generates g-Fe
2O
3Nanocrystal;
(2) add again ZnCl
2With NaOH solution, make its g-Fe
2O
3The nanocrystal surface produces the modulation reaction, at g-Fe
2O
3The crystal grain extension generates ZnFe
2O
4Layer, and at ZnFe
2O
4Form again Zn (OH) on layer
2Outermost layer, obtain composite nano particle;
The nanoparticle of prepared acquisition is the multilayered structure that different magnetic substances consist of, and the dispersiveness of this kind magnetic nanometer particles better.
2. preparation method according to claim 1, is characterized in that, the specific magnetising moment of the NaOH modulation final products by adding different amounts in the composite nano particle synthesis step.
3. preparation method according to claim 1 and 2, is characterized in that, the concrete mode of the presoma preparation of the described the first step is as follows:
(1) FeCl of preparation 0.5-4M concentration
3The aqueous solution, ie in solution 1, the Mg (NO of 1-3M concentration
3)
2The aqueous solution, ie in solution 2; According to every liter of Mg (NO
3)
2The aqueous solution adds the ratio of 3-10molHCl to add HCl in Mg (NO
3)
2In solution, prepare in addition the NaOH aqueous solution of 0.1-2M concentration, ie in solution 3;
(2) mol ratio according to Fe, Mg is that 1-3:1 measures solution 1 and solution 2, solution 1 is poured into obtained solution 2' in solution 2; Volume ratio according to solution 2' and solution 3 is that 1:10 chooses solution 3 again, under agitation condition, solution 3 is poured into fast and is obtained solution 3' in solution 2';
(3) under agitation heated solution 3' to boiling, keeps boiling 1-8 minute, and then stopped heating, naturally cool to room temperature, and along with temperature descends, presoma is Precipitation gradually, until precipitin reaction finishes;
(4) clear liquid is outwelled in centrifugation, obtains presoma.
4. preparation method according to claim 1 and 2, is characterized in that, the concrete grammar of the composite nano particle preparation of described second step is as follows:
The FeCl of preparation 0.1-4M
2The aqueous solution, ie in solution 4, the ZnCl of 0.2-6M
2The aqueous solution, ie in solution 5, the NaOH aqueous solution of 0.1-7M, ie in solution 6;
A, g-Fe
2O
3Synthesizing of nanoparticle
(1) presoma that obtains is poured in solution 4, got solution 4';
(2) solution 4' under agitation is heated to boiling, and keeps boiling 5-30 minute;
B. surface modulation
(3) add successively solution 5 and solution 6;
(4) continue boiling 5-30 minute, then naturally cool to room temperature, precipitation is precipitated thing after finishing;
C, cleaning, drying
(1) take acetone as scavenging solution, the add-on of acetone is 4-6 times of throw out volume, and centrifugation after fully stirring repeats 3-5 time;
(2) product after cleaning changes in vacuum drying oven, obtains anhydrous composite magnetic nanoparticle after 24 hours.
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|---|---|---|---|
| CN201310078459.9A CN103112902B (en) | 2013-03-12 | 2013-03-12 | Method for preparing composite nanoparticles with adjustable magnetism |
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|---|---|---|---|
| CN201310078459.9A CN103112902B (en) | 2013-03-12 | 2013-03-12 | Method for preparing composite nanoparticles with adjustable magnetism |
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| CN103112902A true CN103112902A (en) | 2013-05-22 |
| CN103112902B CN103112902B (en) | 2014-12-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106268830A (en) * | 2016-08-08 | 2017-01-04 | 辽宁大学 | A kind of Fe2o3/ ZnFe2o4composite photo-catalyst and its preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497463A (en) * | 2009-03-06 | 2009-08-05 | 西南大学 | Method for preparing gamma-Fe2O3 nanoparticle by two-step precipitation |
| CN101887791A (en) * | 2010-06-30 | 2010-11-17 | 西南大学 | Preparation method of Zn-gamma-Fe2O3-based magnetic gel |
| CN102910682A (en) * | 2012-09-29 | 2013-02-06 | 西南大学 | Preparation method of gamma-Fe2O3/ZnFe2O4 magnetic composite nano particle |
-
2013
- 2013-03-12 CN CN201310078459.9A patent/CN103112902B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497463A (en) * | 2009-03-06 | 2009-08-05 | 西南大学 | Method for preparing gamma-Fe2O3 nanoparticle by two-step precipitation |
| CN101887791A (en) * | 2010-06-30 | 2010-11-17 | 西南大学 | Preparation method of Zn-gamma-Fe2O3-based magnetic gel |
| CN102910682A (en) * | 2012-09-29 | 2013-02-06 | 西南大学 | Preparation method of gamma-Fe2O3/ZnFe2O4 magnetic composite nano particle |
Non-Patent Citations (3)
| Title |
|---|
| B. MARTINEZ ET AL.: "Low Temperature Surface Spin-Glass Transition in γ-Fe2O3 Nanoparticles", 《PHYSICAL REVIEW LETTERS》 * |
| 文榜才等: "ZnFe2O4基磁凝胶的制备及磁性 ", 《西南大学学报(自然科学版)》, vol. 31, no. 7, 31 July 2009 (2009-07-31), pages 95 - 100 * |
| 文榜才等: "ZnFe2O4基磁凝胶的制备及磁性", 《西南大学学报(自然科学版)》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106268830A (en) * | 2016-08-08 | 2017-01-04 | 辽宁大学 | A kind of Fe2o3/ ZnFe2o4composite photo-catalyst and its preparation method and application |
| CN106268830B (en) * | 2016-08-08 | 2019-01-01 | 辽宁大学 | A kind of Fe2O3/ZnFe2O4Composite photo-catalyst and its preparation method and application |
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