CN103112902B - Method for preparing composite nanoparticles with adjustable magnetism - Google Patents
Method for preparing composite nanoparticles with adjustable magnetism Download PDFInfo
- Publication number
- CN103112902B CN103112902B CN201310078459.9A CN201310078459A CN103112902B CN 103112902 B CN103112902 B CN 103112902B CN 201310078459 A CN201310078459 A CN 201310078459A CN 103112902 B CN103112902 B CN 103112902B
- Authority
- CN
- China
- Prior art keywords
- solution
- presoma
- aqueous solution
- preparation
- nano particle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Hard Magnetic Materials (AREA)
- Compounds Of Iron (AREA)
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 modulation of nanoparticle is synthesized, by controlling the alkaline condition of solution with the method for the different composite nano particle of the preparation specific magnetising moment.
Background technology
Nanoparticle is the nano material that three dimension scale is all less than 100nm, and in inorganic or organic materials, many physical phenomenons have 1 to 100nm characteristic length scale.Magnetic nanometer particles is important functional materials, has important value in fundamental research and applied research.For example, magnetic nanometer particles is scattered in the magnetic liquid forming in silicone oil and can be used as a kind of well sealing material.
Composite nano materials be at least one be two-phase or multiphase material of nanoscale mutually.The combination of different physics or chemical property causes matrix material may have strange character completely.Composite nano particle is generally inclusion.The composite nano particle with gradient magnetic being made up of strong magnetic (ferromagnetic or Ferrimagnetic) core and weak magnetic (antiferromagnetic or paramagnetic) shell may have good dispersiveness.One of important channel of preparing nucleocapsid structure composite nano particle is to carry out surface modulation in the body material building-up process of heart core portion, thereby forms heterogeneous upper layer.G-Fe
2o
3belong to ferrimagnetism material, ZnFe
2o
4belong to antiferromagnetic substance, Zn (OH)
2belong to paramagnetic substance.Prepare the g-Fe of the different specific magnetising moment by controlling synthesis condition
2o
3/ ZnFe
2o
4/ Zn (OH)
2the synthetic method of composite nano particle have not been reported.
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:
A preparation method for the composite nano particle that magnetic is adjustable,
The first step: presoma preparation
In alkaline medium, co-precipitation Fe
3+-Mg
2+the mixture of the aqueous solution, obtains oxyhydroxide presoma;
Second step: composite nano particle synthetic
(1) by presoma at FeCl
2in solution, there is chemical induction phase transformation, generate g-Fe
2o
3nanocrystal;
(2) add again ZnCl
2with NaOH solution, make its g-Fe
2o
3nanocrystal surface produces modulation reaction, at g-Fe
2o
3crystal grain extension generates ZnFe
2o
4layer, and at ZnFe
2o
4on layer, form again Zn (OH)
2outermost layer, obtain composite nano particle;
The nanoparticle of prepared acquisition is the multilayered structure that different magnetic substances form, and the dispersiveness of this kind of magnetic nanometer particles is better.
The concrete grammar that wherein prepared by the presoma of the first step 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) according to Fe, Mgmol than measuring appropriate solution 1 and solution 2 for 1-3:1; Solution 1 is poured into and in solution 2, obtained solution 2'.Be that 1:10 chooses appropriate solution 3 according to the volume ratio of solution 2' and solution 3 again.Under agitation condition, solution 3 is poured into fast and in solution 2', obtained solution 3'.
(3) under agitation heat 3' to boiling.Keep boiling 1-8 minute, then stop heating, naturally cool to room temperature, along with temperature declines, presoma is Precipitation gradually.After two hours, precipitin reaction finishes.
(4) centrifugation, outwells clear liquid, obtains presoma.
Concrete grammar prepared by the composite nano particle of second step is as follows:
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 (solution 6) of 0.1-7M.Can be divided into g-Fe by precursor synthesis composite nano particle
2o
3nanocrystalline particulate forms and two processes of surface modulation:
A, g-Fe
2o
3synthesizing of nanoparticle
(1) presoma the first step precipitin reaction being obtained is poured in solution 4, obtains solution 4';
(2) solution 4' is under agitation 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, dry
(1) taking 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 is proceeded in vacuum drying oven.After 24 hours, obtain anhydrous composite magnetic nanoparticle.
Present method raw materials cost is low, processing condition are gentle, preparation process easy handling, and prepared Magnetic nano composite particles is by Zn (OH)
2the g-Fe of parcel
2o
3/ ZnFe
2o
4mULTILAYER COMPOSITE nanoparticle, its magnetic distribution gradient from inside to outside, this kind of nanoparticle size is little, good dispersity.
Brief description of the drawings
Fig. 1 is the magnetzation curve of the composite nano particle prepared of this law embodiment 1.
Fig. 2 is the transmission electron microscope picture of the composite nano particle prepared of this law embodiment 1.
Fig. 3 is the magnetzation curve of the composite nano particle prepared of this law embodiment 2.
Fig. 4 is the transmission electron microscope picture of the composite nano particle prepared of this law embodiment 2.
Fig. 5 is the magnetzation curve of the composite nano particle prepared of this law embodiment 3.
Fig. 6 is the transmission electron microscope picture of the composite nano particle prepared of this law embodiment 3.
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 stop heating.
(4) naturally cool to room temperature.The complete Precipitation of presoma after approximately 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) pour the presoma synthetic the first step into solution 4, obtain 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.Stop heating, be cooled to room temperature.Within 2 hours, postprecipitation process finishes completely.
Three, clean, be dried
(1) outwell the upper clear supernate after Precipitation, mix with it with the acetone that volume is 5 times of throw outs.After fully stirring, carry out centrifugation, this step repetition 3 times.
(2) precipitation after cleaning is proceeded in vacuum drier, after 24 hours, obtain dry anhydrous composite nano particle.
As shown in Figure 1, its form as shown in Figure 2 for the ratio magnetzation curve of the synthetic nanoparticle of embodiment 1.
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 stop heating.
(4) naturally cool to room temperature.The complete Precipitation of presoma after approximately 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) pour the presoma synthetic the first step into solution 4, obtain 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.Stop heating, be cooled to room temperature.Within 2 hours, postprecipitation process finishes completely.
Three, clean, be dried
With embodiment 1 same operation.
As shown in Figure 3, its form as shown in Figure 4 for the ratio magnetzation curve of the synthetic nanoparticle of embodiment 2.
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) pour the presoma synthetic the first step into solution 4, obtain 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.Stop heating, be cooled to room temperature.Within 2 hours, postprecipitation process finishes completely.
Three, clean, be dried
With embodiment 1 same operation.
As shown in Figure 5, its form as shown in Figure 6 for the ratio magnetzation curve of the synthetic nanoparticle of embodiment 3.
Claims (2)
1. the composite nano particle preparation method of Adjustable magnetic, comprises the steps:
The first step: presoma preparation; In alkaline medium, co-precipitation Fe
3+-Mg
2+the mixture of the aqueous solution, obtains oxyhydroxide presoma;
The 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 3-10mol HCl 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;
Be that 1-3:1 measures solution 1 and solution 2 according to the mol ratio of Fe, Mg, solution 1 is poured into and in solution 2, obtained solution 2'; Be that 1:10 chooses solution 3 according to the volume ratio of solution 2' and solution 3 again, under agitation condition, solution 3 poured into fast and in solution 2', obtained solution 3';
Under agitation heated solution 3', to boiling, keeps boiling 1-8 minute, then stops heating, naturally cools to room temperature, and along with temperature declines, presoma is Precipitation gradually, until precipitin reaction finishes;
Centrifugation, outwells clear liquid, obtains presoma;
Second step: composite nano particle synthetic
(1) by presoma at FeCl
2in solution, there is chemical induction phase transformation, generate g-Fe
2o
3nanocrystal;
(2) add again ZnCl
2with NaOH solution, make its g-Fe
2o
3nanocrystal surface produces modulation reaction, at g-Fe
2o
3crystal grain extension generates ZnFe
2o
4layer, and at ZnFe
2o
4on layer, form again Zn (OH)
2outermost layer, obtain composite nano particle;
The concrete grammar of 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
The presoma obtaining is poured in solution 4, obtained solution 4';
Solution 4' is under agitation heated to boiling, and keeps boiling 5-30 minute;
B. surface modulation
Add successively solution 5 and solution 6;
Continue boiling 5-30 minute, then naturally cool to room temperature, after precipitation finishes, be precipitated thing;
C, cleaning, dry
Taking 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;
Product after cleaning is proceeded in vacuum drying oven, after 24 hours, obtain anhydrous composite magnetic nanoparticle;
The nanoparticle of prepared acquisition is the multilayered structure that different magnetic substances form, and the dispersiveness of this kind of magnetic nanometer particles is better.
2. preparation method according to claim 1, is characterized in that, in composite nano particle synthesis step by adding the specific magnetising moment of NaOH modulation final products of different amounts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310078459.9A CN103112902B (en) | 2013-03-12 | 2013-03-12 | Method for preparing composite nanoparticles with adjustable magnetism |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310078459.9A CN103112902B (en) | 2013-03-12 | 2013-03-12 | Method for preparing composite nanoparticles with adjustable magnetism |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103112902A CN103112902A (en) | 2013-05-22 |
| CN103112902B true CN103112902B (en) | 2014-12-03 |
Family
ID=48411312
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310078459.9A Expired - Fee Related CN103112902B (en) | 2013-03-12 | 2013-03-12 | Method for preparing composite nanoparticles with adjustable magnetism |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103112902B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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 (8)
| Title |
|---|
| #1048577 * |
| #305 * |
| .《西南大学学报(自然科学版)》.2009,第31卷(第7期),第95-100页. * |
| B. Martı * |
| B. Mart& * |
| nez et al..Low Temperature Surface Spin-Glass Transition in γ-Fe2O3 Nanoparticles.《PHYSICAL REVIEW LETTERS》.1998,第80卷(第1期),第181-184页. * |
| 文榜才等.ZnFe2O4基磁凝胶的制备及磁性􀀁 * |
| 文榜才等.ZnFe2O4基磁凝胶的制备及磁性& * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103112902A (en) | 2013-05-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Mosleh et al. | Effect of annealing temperature on structural and magnetic properties of BaFe12O19 hexaferrite nanoparticles | |
| Stefan et al. | Synthesis and characterization of Fe3O4–TiO2 core-shell nanoparticles | |
| Sivakumar et al. | Preparation of sheet like polycrystalline NiFe2O4 nanostructure with PVA matrices and their properties | |
| Anandha Babu et al. | Microwave synthesis and effect of CTAB on ferromagnetic properties of NiO, Co 3 O 4 and NiCo 2 O 4 nanostructures | |
| Sharma et al. | Physical and magnetic properties of manganese ferrite nanoparticles | |
| CN101497463B (en) | Method for preparing gamma-Fe2O3 nanoparticle by two-step precipitation | |
| Zhao et al. | Effect of surfactant amount on the morphology and magnetic properties of monodisperse ZnFe2O4 nanoparticles | |
| Chen et al. | Fabrication of Nd-doped Ni–Zn ferrite/multi-walled carbon nanotubes composites with effective microwave absorption properties | |
| Roman et al. | Structural changes of cerium doped copper ferrites during sintering process and magneto-electrical properties assessment | |
| Shobana et al. | Preparation and characterisation of NiCo ferrite nanoparticles | |
| Javadi et al. | Conventional versus microwave combustion synthesis of CoFe 2 O 4 nanoparticles | |
| Sun et al. | Hydrothermal synthesis of magnetite: Investigation of influence of aging time and mechanism | |
| Lwin et al. | Influence of pH on the physical and electromagnetic properties of Mg–Mn ferrite synthesized by a solution combustion method | |
| Fu et al. | Preparation and magnetic properties of SrFe12O19/SiO2 nanocomposites with core–shell structure | |
| Atabaev et al. | Fabrication of bifunctional core-shell Fe 3 O 4 particles coated with ultrathin phosphor layer | |
| Puspitasari et al. | Effects of various sintering conditions on the structural and magnetic properties of zinc ferrite (ZnFe 2 O 4) | |
| Meng et al. | Effect of In3+ substitution on structural and magnetic properties of Ni ferrite nanoparticles | |
| Wang et al. | Synthesis of monodisperse nanocrystals of high crystallinity magnetite through solvothermal process | |
| Raghavender | Synthesis and characterization of cobalt ferrite nanoparticles | |
| Qiu et al. | Facile synthesis of yolk-shell pompon-like Fe@ void@ CeO2@ Ni nanospheres with enhanced microwave absorption properties | |
| Manikandan et al. | Comparative study of pure and Ni-doped ZnFe2O4 nanoparticles for structural, optical and magnetic properties | |
| Xue et al. | Preparation of core‐shell Zn‐doped CoFe2O4 cubes@ CNT composites and their absorbing performances | |
| CN103112902B (en) | Method for preparing composite nanoparticles with adjustable magnetism | |
| Zheng et al. | Synthesis of hexagonal CoFe2O4/ZnO nanoparticles and their electromagnetic properties | |
| Mehran et al. | Investigation of structural and magnetic effects of cobalt doping in ZnFe 2 O 4 nanoparticles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20141203 Termination date: 20180312 |