CN101538691A - Method for preparing FePt:RE amorphous alloy nano material mixed with rare earth elements - Google Patents
Method for preparing FePt:RE amorphous alloy nano material mixed with rare earth elements Download PDFInfo
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- CN101538691A CN101538691A CN200910049489A CN200910049489A CN101538691A CN 101538691 A CN101538691 A CN 101538691A CN 200910049489 A CN200910049489 A CN 200910049489A CN 200910049489 A CN200910049489 A CN 200910049489A CN 101538691 A CN101538691 A CN 101538691A
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Abstract
The invention discloses a method for preparing FePt:RE amorphous alloy nano material mixed with rare earth elements, platinum-containing inorganic salt/platinum-containing composition, iron-containing inorganic salt/iron-containing composition and water soluble salt of RE(RE=Eu, Dy, Ce) are used as the reaction precursor, the reaction precursor, organic solvent and phase transfer catalyst crown ether are put into a high pressure kettle, and the needed product is obtained through reaction by making use of the phase transfer among the reactants and the coreduction of the reaction precursor and taking oleic acid as the stabilizer. Based on the invention, alloy nano particles of FePt:Ce, FePt:Dy and FePt:Eu with the particle diameter being 3-5nm can be synthesized, the synthesized alloy nano particles have chemical out-of sequence fcc structure, the amorphous state inclination of the alloy is reinforced by mixing Eu, and the coercive force is greatly enhanced. The alloy nano particles of FePt:Ce and FePt:Dy are processed by backfire at 600 DEG C, the structure thereof carries out phase variation on sequenced L10. At the same time, with the enhanced coercive force, the thermal stability of the FePt:Eu alloy is reinforced by mixing Eu, thus having certain phase variation inhibition effect; in addition, the FePt alloy nano particles are caused to have fluorescence by mixing rare earth elements.
Description
Technical field
The invention belongs to the material technology field, be specifically related to a kind of new have epipolic doped with rare-earth elements RE (RE=Eu, Dy, the preparation method of FePt alloy nano particle Ce).
Background technology
High speed development along with electronics and information industry, demand to high-density, jumbo magnetic recording device is more and more stronger, the research of super-high density magnetic record becomes an important front edge problem of magnetics material and engineering research, has shown very tempting application prospect.Wherein the FePt nano structural material has good chemical stability and higher magnetocrystalline anisotropy, demonstrates huge application potential in the Ultrahigh-Density Data Storage field.L
10The FePt alloy of phase has very high magnetocrystalline anisotropy, and its monadic magnetocrystalline anisotropy constant K u is (6.6～10) * 10
7Erg/cm
2, exceed tens of times than the anisotropy constant of the Co based alloy magnetic recording medium of current use.Thereby be considered to the super-high density magnetic recording media material of potentialization.
The adding of the third element is having significant effect to the FePt alloy nano particle aspect the phase transition, such as: Au, Ag, Sb and Ni, they are by separating the third yuan generation effect usually under the pyritous condition, because rare earth element has special f electronic structure, 5s and 5p electronics make the 4f electronics of internal layer not be subjected to the influence of environment, therefore, rear-earth-doped special light, electricity, the magnetic phenomenon of showing.Eu
2+Be important changeable valence rare earth ion, have the d-f transition of permission, the fluorescent emission wider distribution both can be made good activator, can be used as again the effective sensitizing agent of other ionoluminescence enhanced.Dy
3+As a kind of catalysis doping agent of different inorganic matrixes commonly used, make these matrix suitably regulating under the condition of gold-tinted and blue emission, launch white light.These two kinds of rare earth ions all are widely used in the luminescent material development.Therefore in order further to open up the magnetic and the optical property of FePt alloy nano particle, this patent is introduced the FePt alloy system with rare earth element, synthesizes FePt:RE (RE=Eu, Dy, Ce) alloy nano particle of a series of doped with rare-earth elements.
Nano material has the not available unusual or unusual physics of traditional material, chemical property, can produce four big effects: small-size effect, quantum effect (containing macro quanta tunnel effect), surface effects and interfacial effect.Use our synthetic method, it is good to prepare monodispersity, uniform particle diameter have a rare earth doped FePt alloy nano particle of fluorescence, thereby have excellent physico-chemical property.
The method for preparing rare earth doped monodispersity FePt alloy in the bibliographical information is mainly the physics method.This method mainly be utilize physical sputtering method with rare earth doped in the FePt alloy.Problems such as these methods all exist equipment, technical requirements harshness, and the gained size of particles is bigger, and it is inhomogeneous to mix.
Summary of the invention
The object of the present invention is to provide a kind of rare earth doped FePt Nanoalloy preparation method of fluorescence that has, and expectation can be generalized to industrial application.
A kind of preparation method of FePt Nanoalloy of doped with rare-earth elements, with platiniferous inorganic salt/contain platinum complex, iron content inorganic salt/contain iron complex and RE (RE=Eu, Dy, Ce) water-soluble salt is as the reaction precursor body, pre-reaction material, organic solvent, phase-transfer catalyst crown ether are placed in the autoclave, utilize the phase transition between the reactant and the coreduction of pre-reaction material, reaction makes desired product as stablizer with oleic acid.
Further, in the autoclave, under 120 ℃-180 ℃, react and made desired product in 8-15 hour.
Described water-soluble salt comprises nitrate or muriate.
May further comprise the steps:
(1) (RE=Eu, Dy Ce) are dissolved in the organic solvent, add sodium oleate and the DB24C8 (C suitable with molysite platinum salt amount successively with platiniferous inorganic salt/contain platinum complex and iron content inorganic salt/contain iron complex and water miscible RE inorganic salt
24H
32O
8, crown ether), be stirred to solid and dissolve fully; The mol ratio of platiniferous inorganic salt/contain platinum complex, iron content inorganic salt/contain iron complex, RE inorganic salt is (4.5～5.4): 4.5: (1～0.1); The mol ratio of total amount of sodium oleate and molysite and platinum salt is 5: 1～10: 1; The mol ratio of total amount of substance of hexichol crown ether and molysite and platinum salt is 1: 30～1: 100; The mol ratio of total amount of substance of organic solvent and molysite and platinum salt is 30: 1～80: 1;
(2) polyvalent alcohol and oleic mixing solutions are joined in the resulting mixture of step (1), whole mixed system is moved into autoclave, reacted 15 hours down at 160 ℃; Reaction is cooled to room temperature after finishing, washing, and centrifugation obtains final product black alloy nanoparticle; Wherein propylene glycol and oleic volume ratio are 2: 1～3: 1; The mol ratio of propylene glycol and molysite and the total amount of platinum salt is 30: 1～80: 1;
Polyvalent alcohol described in the step (2) comprises ethylene glycol or propylene glycol.
Described platiniferous inorganic salt be in the platiniferous water-soluble inorganic salts such as Platinic chloride or platinum dichloride any, platiniferous organic salt is that dichloride dicyan phenylbenzene closes in the water-soluble complexes of platinum (II) or acetyl acetone platinum platinum such as (II) any, the iron content inorganic salt comprise water-soluble iron content inorganic salt such as iron protochloride, iron(ic) chloride for the iron content inorganic salt, iron content organic salt be in ironic oxalate, acetyl acetone iron (II) or the acetyl acetone iron water-soluble iron content organic salts such as (III) any; Described RE is Eu, Dy, in the water miscible nitrate of Ce or the muriate any one.
Stirring described in the step (1) is ultrasonic concussion or magnetic agitation.
Centrifugation rotating speed described in the step (2) is 3000-5000 rev/min, and the time is 10-20 minute.
Utilize the inventive method to prepare that monodispersity is good, the FePt:RE nanoparticle of uniform particle diameter, the FePt particle of doping Eu has formed uniformly, the club shaped structure of high length-diameter ratio; Doping Dy, the method for Ce has obtained that monodispersity is good, the alloy nano particle of uniform particle diameter, has excellent physico-chemical property.For example can be applied to have fluorescence etc. in the hard disk HAMR technology.
The inventive method is easy to operate, easy to control, and the product of preparing can be prepared alloy firm as LB, impregnating method by further operation.Structure, pattern, composition to the inventive method products therefrom characterize, can select X-ray powder diffraction (XRD), projection electron microscope (TEM), fourier transform infrared spectroscopy (FTIR), differential scanning calorimeter (DSC), x-ray photoelectron spectroscopy (XPS), transmission electricity border (TEM) etc. respectively for use, XRD result shows crystal formation, size-grade distribution and the main component of product, SEM, TEM shows particle diameter and whole pattern, the result of FTIR checking XRD and the kind and the content of particle surface bag addendum.It is elementary composition that XPS detects microcell, the result of evidence XRD.
The present invention has the following advantages:
1. effectively synthesize the about 3-5nm of particle diameter, and the rare earth doped FePt:RE alloy nano particle of narrow diameter distribution.
2.Eu doping, the amorphous tendency of FePt:Eu is increased, the thermostability of alloy improves, and plays the effect that suppresses phase transformation.Obtained long bar-shaped alloy nano rod simultaneously.
3. synthetic FePt:Ce of institute and FePt:Dy alloy nano particle monodispersity are good, uniform particle diameter.
4. the FePt:RE amorphous alloy nano particle that is condensed into has paramagnetism.And the coercive force of FePt:Eu alloy nano particle increases greatly.The saturation magnetization of the alloy nano particle after the temper and coercive force all improve greatly; Though because of Eu has restraining effect that FePt:Eu is not undergone phase transition to phase transformation, the ordering of alloy also makes the saturation magnetization of material and coercive force improve a lot, and surpass the above two.
5. the test shows of optical property: the doping of rare earth element makes the FePt alloy nanoparticle have fluorescence.
Description of drawings
Fig. 1 is in embodiment 1, example 2, the example 3, adopts Eu, and Dy, the nitrate of Ce are the TEM figure of the FePt:RE of feedstock production.Wherein Fig. 1 (a) is the TEM figure of FePt:Eu; Fig. 1 (b) is the TEM figure of FePt:Dy; Fig. 1 (c) is the TEM figure of FePt:Ce.
Fig. 2 is the fluorescence emission spectrum of the FePt:Dy that obtains among the embodiment 2.
Embodiment
The present invention is further illustrated below in conjunction with embodiment.
The preparation of embodiment 1:FePt:Eu alloy magnetic nano-particle
The first step is with 0.031mmol H
2PtCl
66H
2O and 0.031mmol Fe
2(C
2O
4)
35H
2O and 0.007mmolEu (NO
3)
3Be dissolved in fully in the 2ml dehydrated alcohol, add 0.2g sodium oleate and 0.011molDB24C8 then successively, ultrasonic concussion was stirred 10 minutes, dissolved fully to solid.
In second step, add 4ml 1, the oleic mixing solutions of 2-propylene glycol and 2ml, then whole mixed system is transferred in the autoclave, be warming up to 423K, in retort furnace, under the condition of 423K, be incubated 15 hours with 2 ℃/minute speed, reaction is cooled to room temperature after finishing.
The 3rd step, use the sedimentary particle in dehydrated alcohol and distilled water wash reactor bottom successively repeatedly, and under 5000 rev/mins speed centrifugal 10 minutes, at last with the nanoparticle that obtains vacuum drying oven inner drying 2 hours.Product is analyzed.
The TEM electromicroscopic photograph shows that product is the nanometer rod of monodispersity among Fig. 1 (a), has bigger length-to-diameter ratio.
The preparation of embodiment 2:FePt:Dy alloy magnetic nano-particle
With 0.031mmol H
2PtCl
66H
2O and 0.031mmol Fe
2(C
2O
4)
35H
2O and 0.007mmol Dy (NO
3)
3Be dissolved in fully in the 2ml dehydrated alcohol, add 0.2g sodium oleate and 0.011molDB24C8 then successively, ultrasonic concussion was stirred 10 minutes, dissolved fully to solid.Add 4ml 1, the oleic mixing solutions of 2-propylene glycol and 2ml is transferred to whole mixed system in the autoclave then, reacts 15 hours under the condition of 423K in retort furnace, and reaction is cooled to room temperature after finishing.All the other press embodiment 1 described step operation.The TEM electromicroscopic photograph shows that product is amorphous nano level particle among Fig. 1 (b), and particle diameter is little and have a monodispersity.When exciting at the 397nm place among Fig. 2, occurred two emission peaks of 467nm and 597nm on the emmission spectrum of FePt:Dy, these two peaks correspond respectively to Dy
3+4F
9/2-6H
15/2With 4F
9/2-6H
13/2The transition emission peak, wherein the peak of 467nm is the non-sensitive transition peak of blue light, the responsive transition peak of the corresponding gold-tinted of 597nm.Therefore, the adding of rare earth element Dy makes FePt alloy magnetic nano-particle have fluorescence.
The preparation of embodiment 3:FePt:Ce alloy magnetic nano-particle
With 0.031mmol H
2PtCl
66H
2O and 0.031mmol Fe
2(C
2O
4)
35H
2O and 0.007mmol Ce (NO
3)
3Be dissolved in fully in the 2ml dehydrated alcohol, add 0.2g sodium oleate and 0.011molDB24C8 then successively, press embodiment 2 described step reaction.The TEM electromicroscopic photograph shows that product is amorphous nano level particle among Fig. 1 (c), and particle diameter is little and have a monodispersity.
Products therefrom magnetic behavior characterization data in table 1 embodiment 1, example 2, the example 3
| Alloy nano particle | Coercive force (Oe) | Saturation magnetization (emu/g) |
| FePt:Eu | 310 | 0.027 |
| FePt:Dy | 17.0 | 0.14 |
| FePt:Ce | 24.0 | 0.40 |
| FePt:Eu (after the tempering) | 527 | 4.39 |
| FePt:Dy (after the tempering) | 166 | 5.46 |
| FePt:Ce (after the tempering) | 330 | 4.17 |
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.The person skilled in the art obviously can easily make various modifications to these embodiment, and needn't pass through performing creative labour being applied in the General Principle of this explanation among other embodiment.Therefore, the invention is not restricted to the embodiment here, those skilled in the art should be within protection scope of the present invention for improvement and modification that the present invention makes according to announcement of the present invention.
Claims (8)
1, a kind of preparation method of FePt Nanoalloy of doped with rare-earth elements is characterized in that: with platiniferous inorganic salt/contain platinum complex, iron content inorganic salt/contain iron complex and RE (RE=Eu, Dy, water-soluble salt Ce)
As the reaction precursor body, pre-reaction material, organic solvent, phase-transfer catalyst crown ether are placed in the autoclave, utilize the phase transition between the reactant and the coreduction of pre-reaction material, reaction makes desired product as stablizer with oleic acid.
2, preparation method according to claim 1 is characterized in that: in the autoclave, under 120 ℃-180 ℃, react and made desired product in 8-20 hour.
3, preparation method according to claim 1 is characterized in that: described water-soluble salt comprises nitrate or muriate.
4, preparation method according to claim 1 is characterized in that: may further comprise the steps:
(1) (RE=Eu, Dy Ce) are dissolved in the organic solvent, add sodium oleate and DB24C8 (C successively with platiniferous inorganic salt/contain platinum complex and iron content inorganic salt/contain iron complex and water miscible RE inorganic salt
24H
32O
8, crown ether), be stirred to solid and dissolve fully; The mol ratio of platiniferous inorganic salt/contain platinum complex, iron content inorganic salt/contain iron complex, RE inorganic salt is (4.5～5.4): 4.5: (1～0.1); The mol ratio of total amount of sodium oleate and molysite and platinum salt is 5: 1～10: 1; The mol ratio of total amount of substance of hexichol crown ether and molysite and platinum salt is 1: 30～1: 100; The mol ratio of total amount of substance of organic solvent and molysite and platinum salt is 30: 1～80: 1;
(2) polyvalent alcohol and oleic mixing solutions are joined in the resulting mixture of step (1), whole mixed system is moved into autoclave, reacted 15 hours down at 160 ℃; Reaction is cooled to room temperature after finishing, washing, and centrifugation obtains final product black alloy nanoparticle; Wherein propylene glycol and oleic volume ratio are 2: 1～3: 1; The mol ratio of propylene glycol and molysite and the total amount of platinum salt is 30: 1～80: 1;
5, preparation method according to claim 4 is characterized in that: the polyvalent alcohol described in the step (2) comprises ethylene glycol or propylene glycol.
6, according to claim 1 or 4 described preparation methods, it is characterized in that: described platiniferous inorganic salt be in Platinic chloride or the platinum dichloride any, platiniferous organic salt is that dichloride dicyan phenylbenzene closes in platinum (II) or the acetyl acetone platinum (II) any, the iron content inorganic salt be in iron protochloride or the iron(ic) chloride any, iron content organic salt be in ironic oxalate, acetyl acetone iron (II) or the acetyl acetone iron (III) any; Described RE is Eu, Dy, in the water miscible nitrate of Ce or the muriate any one.
7, preparation method according to claim 4 is characterized in that: the stirring described in the step (1) is ultrasonic concussion or magnetic agitation.
8, preparation method according to claim 4 is characterized in that: the centrifugation rotating speed described in the step (2) is 3000-5000 rev/min, and the time is 10-20 minute.
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Cited By (4)
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|---|---|---|---|---|
| CN102626786A (en) * | 2012-03-30 | 2012-08-08 | 武汉理工大学 | Preparing method of FePt/graphene composite nano materials |
| CN105833862A (en) * | 2016-03-31 | 2016-08-10 | 湖南省吉安特技术有限公司 | Preparation method and application of nanometer platinum oxide catalyst |
| CN108060391A (en) * | 2017-12-15 | 2018-05-22 | 桂林电子科技大学 | A kind of method for accelerating FePd film phase transition |
| CN112962122A (en) * | 2021-02-01 | 2021-06-15 | 浙江工业大学 | Preparation method of high-coercivity B-doped FePt film |
-
2009
- 2009-04-17 CN CN2009100494890A patent/CN101538691B/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102626786A (en) * | 2012-03-30 | 2012-08-08 | 武汉理工大学 | Preparing method of FePt/graphene composite nano materials |
| CN102626786B (en) * | 2012-03-30 | 2014-04-09 | 武汉理工大学 | Preparing method of FePt/graphene composite nano materials |
| CN105833862A (en) * | 2016-03-31 | 2016-08-10 | 湖南省吉安特技术有限公司 | Preparation method and application of nanometer platinum oxide catalyst |
| CN105833862B (en) * | 2016-03-31 | 2018-09-28 | 湖南省吉安特技术有限公司 | A kind of preparation method and application of nano oxidized platinum catalyst |
| CN108060391A (en) * | 2017-12-15 | 2018-05-22 | 桂林电子科技大学 | A kind of method for accelerating FePd film phase transition |
| CN108060391B (en) * | 2017-12-15 | 2019-12-27 | 桂林电子科技大学 | Method for accelerating phase transition of FePd thin film |
| CN112962122A (en) * | 2021-02-01 | 2021-06-15 | 浙江工业大学 | Preparation method of high-coercivity B-doped FePt film |
| CN112962122B (en) * | 2021-02-01 | 2022-03-15 | 浙江工业大学 | Preparation method of high-coercivity B-doped FePt film |
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| CN101538691B (en) | 2011-06-22 |
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