CN105984903B - A kind of MnFe2O4The preparation method of nano magnetic material - Google Patents
A kind of MnFe2O4The preparation method of nano magnetic material Download PDFInfo
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Abstract
The invention discloses a kind of MnFe2O4The preparation method of nano magnetic material, manganous salt sample, trivalent iron salt sample are weighed by specified quantitative, as solvent and added after oleyl amine and oleic acid forms mixed liquor, mixed liquor is heated, heating process is in N using benzyl ether2Carried out under atmosphere protection, the microcosmic upper MnFe in symmetrical structure can be obtained2O4Nano magnetic material, by selecting suitable heating parameters, three degree of symmetrical, four degree of symmetrical, six degree of symmetrical, MnFe of rhombic symmetry can be obtained2O4Nano magnetic material.The invention provides a kind of MnFe2O4Nano magnetic material preparation method, the MnFe prepared2O4Nano magnetic material has good symmetry；The ran of particle diameter about 50, close to protein and the size of virus, and dispersiveness is preferably.
Description
Technical field
The present invention relates to MnFe2O4Preparation method of nano material field, be specifically a kind of three degree it is symmetrical, four degree symmetrically, six degree
Symmetrically, the MnFe of rhombic symmetry2O4The preparation method of nano magnetic material.
Background technology
Ferrospinel MnFe2O4Due to excellent physicochemical properties, being led in microwave absorption, electromagnetic device etc.
Domain is widely used.Especially, the MnFe of nanoscale2O4After surface modification or functionalization, it is expanded and has been total in magnetic
Shake the application in the fields such as imaging, photocatalysis, lithium battery, ultracapacitor, target administration and the absorption to harmful substance.
The pattern and size of magnetic nano-particle have a significant impact to magnetic property.So far, the MnFe reported2O4Grain
Son pattern have it is spherical, cube, hexagonal shape；By template or seed particles, nano bar-shape, nanofiber can also be prepared
The particle of shape and rugby shape.Vamvakidis, Sun and Gavrilov-Isaac et al. Fe (acac)3With Mn (acac)2
Spherical, hexagonal configuration MnFe has been prepared in thermal decomposition in high-temperature solvent2O4Particle.Lee thermally decomposes legal system with metal oleate
For the MnFe of cubic shape2O4Nano-particle.Li et al. is by the use of metal-nitrate solutions as presoma, using electrospinning system
For MnFe2O4Nanobelt.By the use of Mn and Fe nitrate as raw material, by the use of NaOH as precipitating reagent, by the use of CNT as
Template, MnFe can be prepared2O4Nano wire.
Coprecipitation is also to prepare the conventional method of nano-particle.Hosseini, Ahalya and Gherca et al. metal
Chloride is raw material, and MnFe is prepared using coprecipitation2O4, but prepared particle often random pattern, and assembling existing
As serious.In addition, hydro-thermal method is also to prepare the conventional means of nano-particle.Wang et al. Mn (CH3COO)2·4H2O and
FeCl3·6H2O is raw material, and nano spherical particle is prepared for hydro-thermal method；Sahoo et al. MnCl2And FeCl3For former material
Material, and sodium acetate is added in the solution, then it is prepared for the nanometer spherical particle of particle diameter about 200 with hydro-thermal method.Liu et al. is used
FeCl3·6H2O and MnCl2·4H2O prepares spherical particle as raw material using hydro-thermal method；But Xiong et al. is adopted
With identical raw material and identical hydro-thermal method, the nano-particle of irregular shape is but prepared for.So far, there is not yet three
Degree, four degree of symmetrical and MnFe of hexagonal and rhombic symmetry2O4The report of the preparation of nano-particle.
The content of the invention
It is an object of the invention to provide a kind of MnFe2O4The preparation method of nano magnetic material, to solve prior art preparation
Method can not prepare the symmetrical MnFe of microstructure2O4The problem of nano material.
In order to achieve the above object, the technical solution adopted in the present invention is：
A kind of MnFe2O4The preparation method of nano magnetic material, it is characterised in that：According to manganese：Ferro element mol ratio is 1：2
Manganous salt sample, trivalent iron salt sample are weighed, manganous salt sample will be weighed, trivalent iron salt sample is put into flask, and
Solvent is used as using 400ml benzyl ether in flask, after oleyl amine and each 40ml formation mixed liquor of oleic acid are then added into flask, then
Heated, heating stepses are as follows：
(1) mixed liquor in flask, is heated to 28-32 DEG C and magnetic agitation 28-32min first；
(2) constant temperature 13-17min after and then mixed liquor in flask being heated into 118-122 DEG C, or it is heated to 138-
202 DEG C be cooled to 118-122 DEG C again after constant temperature 13-17min；
(3) constant temperature 1.8-2.2h after mixed liquor in flask then, is heated into 198-202 DEG C；
(4) 0.8-1.2h of constant temperature after mixed liquor in flask finally, is heated into 288-292 DEG C；
Whole heating process is in N2Carried out under atmosphere protection, room temperature is naturally cooled to after the completion of heating, then added appropriate
Alcohol washes are thoroughly limpid up to solution, and the microcosmic upper MnFe in symmetrical structure is obtained after drying2O4Nano magnetic material.
A kind of described MnFe2O4The preparation method of nano magnetic material, it is characterised in that：Select to close in heating stepses
Suitable heating parameters, three degree of symmetrical MnFe are prepared2O4Nano magnetic material, heating stepses are as follows：
(a1) mixed liquor in flask, is heated to 30 DEG C and magnetic agitation 30min first；
(b1) constant temperature 15min after and then mixed liquor in flask being heated into 120 DEG C；
(c1) constant temperature 2h after mixed liquor in flask then, is heated into 200 DEG C；
(d1) constant temperature 1h after mixed liquor in flask finally, is heated into 290 DEG C；
Whole heating process is in N2Carried out under atmosphere protection, room temperature is naturally cooled to after the completion of heating, then added appropriate
Alcohol washes are thoroughly limpid up to solution, and three degree of symmetrical MnFe in microstructure are obtained after drying2O4Nano magnetic material, life
Entitled MFO120.
A kind of described MnFe2O4The preparation method of nano magnetic material, it is characterised in that：Select to close in heating stepses
Suitable heating parameters, four degree of symmetrical MnFe are prepared2O4Nano magnetic material, heating stepses are as follows：
(a2) mixed liquor in flask, is heated to 30 DEG C and magnetic agitation 30min first；
(b2) then by mixed liquor in flask be heated to 140 DEG C or 150 DEG C or 170 DEG C be cooled to 120 DEG C again after
Constant temperature 15min；
(c2) constant temperature 2h after mixed liquor in flask then, is heated into 200 DEG C；
(d2) constant temperature 1h after mixed liquor in flask finally, is heated into 290 DEG C；
Whole heating process is in N2Carried out under atmosphere protection, room temperature is naturally cooled to after the completion of heating, then added appropriate
Alcohol washes are thoroughly limpid up to solution, and four degree of symmetrical MnFe in microstructure are obtained after drying2O4Nano magnetic material, life
Entitled MFO140, either MFO150 or MFO170；
A kind of described MnFe2O4The preparation method of nano magnetic material, it is characterised in that：Select to close in heating stepses
Suitable heating parameters, six degree of symmetrical MnFe are prepared2O4Nano magnetic material, heating stepses are as follows：
(a3) mixed liquor in flask, is heated to 30 DEG C and magnetic agitation 30min first；
(b3) then by mixed liquor in flask be heated to 160 DEG C be cooled to 120 DEG C again after constant temperature 15min；
(c3) constant temperature 2h after mixed liquor in flask then, is heated into 200 DEG C；
(d3) constant temperature 1h after mixed liquor in flask finally, is heated into 290 DEG C；
Whole heating process is in N2Carried out under atmosphere protection, room temperature is naturally cooled to after the completion of heating, then added appropriate
Alcohol washes are thoroughly limpid up to solution, and six degree of symmetrical MnFe in microstructure are obtained after drying2O4Nano magnetic material, life
Entitled MFO160.
A kind of described MnFe2O4The preparation method of nano magnetic material, it is characterised in that：Select to close in heating stepses
Suitable heating parameters, the MnFe of rhombic symmetry is prepared2O4Nano magnetic material, heating stepses are as follows：
(a4) mixed liquor in flask, is heated to 30 DEG C and magnetic agitation 30min first；
(b4) then by mixed liquor in flask be heated to 200 DEG C be cooled to 120 DEG C again after constant temperature 15min；
(c4) constant temperature 2h after mixed liquor in flask then, is heated into 200 DEG C；
(d4) constant temperature 1h after mixed liquor in flask finally, is heated into 290 DEG C；
Whole heating process is in N2Carried out under atmosphere protection, room temperature is naturally cooled to after the completion of heating, then added appropriate
Alcohol washes are thoroughly limpid up to solution, and the MnFe of rhombic symmetry in microstructure is obtained after drying2O4Nano magnetic material, life
Entitled MFO200.
A kind of described MnFe2O4The preparation method of nano magnetic material, it is characterised in that：The manganous salt is divalence
Manganese acetylacetonate.
A kind of described MnFe2O4The preparation method of nano magnetic material, it is characterised in that：The trivalent iron salt is trivalent
Ferric acetyl acetonade.
The invention provides a kind of MnFe2O4Nano magnetic material preparation method, the MnFe prepared2O4Nano-magnetic material
Material has good symmetry；The ran of particle diameter about 50, close to protein and the size of virus；And dispersiveness is preferably, and
By selecting suitable heating parameters, three degree of symmetrical, four degree of symmetrical, six degree of symmetrical, MnFe of rhombic symmetry can be prepared2O4
Nano magnetic material.It is demonstrated experimentally that the MnFe of the shape anisotropy prepared by the present invention2O4Nano-particle, technique is simple, greatly
It is small controllable；The particle obtained has potential using value in fields such as biomedicines.And it is to disclose magnetic nano particle subsystem
The good model system of shape anisotropy effect.
Brief description of the drawings
Fig. 1 is three degree/tetra- degree symmetrical, hexagonals and rhombus MnFe2O4The X-ray diffracting spectrum of nano-magnetic sample.Wherein,
Abscissa is the angle of diffraction, and ordinate is relative intensity.
Fig. 2 is three degree of symmetrical MnFe2O4Nano magnetic material MFO120 TEM figures.It is equilateral triangle as seen from the figure, side
Grow between 20nm-30nm.
Fig. 3 is four degree of symmetrical MnFe2O4Nano magnetic material MFO140 TEM figures.Understand that particle is approximately just by enlarged drawing
Square, the length of side is 50nm or so.
Fig. 4 is four degree of symmetrical MnFe2O4Nano magnetic material MFO150 TEM figures.Understand that particle is approximately just by enlarged drawing
Square, the length of side is 16nm or so.
Fig. 5 is hexagon MnFe2O4Nano magnetic material MFO160 TEM figures.
Fig. 6 is four degree of symmetrical MnFe2O4Nano magnetic material MFO170 TEM figures.Understand that particle is approximately just by enlarged drawing
Square, the length of side is 28nm or so.
Fig. 7 is rhombus MnFe2O4Nano magnetic material MFO200 TEM figures.Understand that particle is approximately rhombus by enlarged drawing,
The length of side is between 22nm-25nm.
Fig. 8 is three degree/tetra- degree symmetrical, hexagonals and rhombus MnFe2O4Nano magnetic material room temperature hysteresis curve collection of illustrative plates.
Embodiment
Embodiment 1：Three degree of symmetrical MnFe2O4The preparation of nano material
According to manganese：Ferro element mol ratio is 1：2, weigh divalence acetylacetone,2,4-pentanedione manganese salt 0.8678g, trivalent acetylacetone iron salt
Sample 2.3965g is dissolved in 100ml benzyl ether organic solvents, while each oleyl amine, oleic acid for adding 20ml, 30 DEG C of magnetic agitations
30mins is then heated to so that acetylacetonate fully melts in organic solvent, and then is warming up to 120 DEG C of constant temperature 15min
200 DEG C of constant temperature 2h, 290 DEG C of constant temperature 1h are finally warming up to, remove heater, naturally cool to room temperature, it is clear to add suitable alcohols
Wash until solution it is thoroughly limpid, be dried to obtain three degree of symmetrical MnFe2O4Nanoparticle sample.
2, four degree of symmetrical MnFe of embodiment2O4The preparation of nano material
According to manganese：Ferro element mol ratio is 1：2, weigh divalence acetylacetone,2,4-pentanedione manganese salt 0.8678g, trivalent acetylacetone iron salt
Sample 2.3965g is dissolved in 100ml benzyl ether organic solvents, while each oleyl amine, oleic acid for adding 20ml, 30 DEG C of magnetic agitations
30mins removes thermal source, is naturally cooling to so that acetylacetonate fully melts in organic solvent, and then is warming up to 140 DEG C
120 DEG C of constant temperature 15min, 200 DEG C of constant temperature 2h are then heated to, be finally warming up to 290 DEG C of constant temperature 1h, remove heater, it is natural
Room temperature is cooled to, the cleaning of addition suitable alcohols is thoroughly limpid up to solution, is dried to obtain four degree of symmetrical MnFe2O4Nano particle
Sample.
Embodiment 3：Four degree of symmetrical MnFe2O4The preparation of nano material
According to manganese：Ferro element mol ratio is 1：2, weigh divalence acetylacetone,2,4-pentanedione manganese salt 0.8678g, trivalent acetylacetone iron salt
Sample 2.3965g is dissolved in 100ml benzyl ether organic solvents, while each oleyl amine, oleic acid for adding 20ml, 30 DEG C of magnetic agitations
30min removes thermal source, is naturally cooling to so that acetylacetonate fully melts in organic solvent, and then is warming up to 150 DEG C
120 DEG C of constant temperature 15min, 200 DEG C of constant temperature 2h are then heated to, be finally warming up to 290 DEG C of constant temperature 1h, remove heater, it is natural
Room temperature is cooled to, the cleaning of addition suitable alcohols is thoroughly limpid up to solution, is dried to obtain four degree of symmetrical MnFe2O4Nano particle
Sample.
Embodiment 4：Four degree of symmetrical MnFe2O4The preparation of nano material
According to manganese：Ferro element mol ratio is 1：2, weigh divalence acetylacetone,2,4-pentanedione manganese salt 0.8678g, trivalent acetylacetone iron salt
Sample 2.3965g is dissolved in 100ml benzyl ether organic solvents, while each oleyl amine, oleic acid for adding 20ml, 30 DEG C of magnetic agitations
30min removes thermal source, is naturally cooling to so that acetylacetonate fully melts in organic solvent, and then is warming up to 170 DEG C
120 DEG C of constant temperature 15min, 200 DEG C of constant temperature 2h are then heated to, be finally warming up to 290 DEG C of constant temperature 1h, remove heater, it is natural
Room temperature is cooled to, the cleaning of addition suitable alcohols is thoroughly limpid up to solution, is dried to obtain four degree of symmetrical MnFe2O4Nano particle
Sample.
Embodiment 5：Hexagon MnFe2O4The preparation of nano material
According to manganese：Ferro element mol ratio is 1：2, weigh divalence acetylacetone,2,4-pentanedione manganese salt 0.8678g, trivalent acetylacetone iron salt
Sample 2.3965g is dissolved in 100ml benzyl ether organic solvents, while each oleyl amine, oleic acid for adding 20ml, 30 DEG C of magnetic agitations
30min removes thermal source, is naturally cooling to so that acetylacetonate fully melts in organic solvent, and then is warming up to 160 DEG C
120 DEG C of constant temperature 15min, 200 DEG C of constant temperature 2h are then heated to, be finally warming up to 290 DEG C of constant temperature 1h, remove heater, it is natural
Room temperature is cooled to, the cleaning of addition suitable alcohols is thoroughly limpid up to solution, is dried to obtain hexagonal MnFe2O4Nano particle sample
Product.
Embodiment 6：Rhombus MnFe2O4The preparation of nano material
According to manganese：Ferro element mol ratio is 1：2, weigh divalence acetylacetone,2,4-pentanedione manganese salt 0.8678g, trivalent acetylacetone iron salt
Sample 2.3965g is dissolved in 100ml benzyl ether organic solvents, while each oleyl amine, oleic acid for adding 20ml, 30 DEG C of magnetic agitations
30min removes thermal source, is naturally cooling to so that acetylacetonate fully melts in organic solvent, and then is warming up to 200 DEG C
120 DEG C of constant temperature 15min, 200 DEG C of constant temperature 2h are then heated to, be finally warming up to 290 DEG C of constant temperature 1h, remove heater, it is natural
Room temperature is cooled to, the cleaning of addition suitable alcohols is thoroughly limpid up to solution, is dried to obtain the MnFe of rhombus2O4Nanoparticle sample.
Embodiment 7:Prepare the sign of gained sample
1st, checking prepares the purity of gained sample
With x-ray diffractometer (XRD；DX-2000 SSC) testing example 1-5 prepare three degree/tetra- degree symmetrically, hexagonals
And rhombus MnFe2O4Nanoparticle sample, corresponding X-ray diffracting spectrum, is shown in Fig. 1, wherein, abscissa is the angle of diffraction, indulges and sits
It is designated as relative intensity..
By the position of each diffraction maximum in Fig. 1 and relative intensity and standard PDF cards (MnFe2O4(No. 731964)) phase
It is pure MnFe made from present invention experiment than understanding2O4Magnetic material.
2nd, the symmetry checking of sample
3rd, three degree/tetra- degree pairs of embodiment 1-6 preparations are characterized using transmission electron microscope (JEOL JEM-2100)
Title, hexagonal and rhombus MnFe2O4Nanoparticle sample, collection of illustrative plates is characterized accordingly, see Fig. 2 to Fig. 7, enlarged drawing (b) in wherein Fig. 2
Understand that particle is equilateral triangle, the length of side is between 20nm-30nm；Fig. 3 enlarged drawings (b) understand that some particles carry wedge angle；
Some particles are approximately square, and catercorner length is about 50nm or so in 70 rans, the i.e. length of side；Fig. 4 enlarged drawings (b)
Understand, particle is approximately square, and the length of side is 16nm or so；Fig. 6 enlarged drawings (b) understand that particle is approximately square, diagonal
Length is about 28nm in 40 rans, the i.e. length of side；Fig. 7 enlarged drawings (b) understand that particle is approximately rhombus, the length of side be 22nm-
Between 25nm.
From Fig. 2 to Fig. 7, the sample of different symmetries can be prepared according to different case study on implementation, respectively three degree/tetra-
Spend the MnFe of symmetrical, hexagonal and rhombus2O4Nano-particle material.
4th, the test of sample magnetic property-room temperature hysteresis curve
Using comprehensive physical property measuring system (PPMS, SQUID, PPMS EC-II) characterize prepared by embodiment 1-5 three degree,
Four degree, six degree and rhombic symmetry MnFe2O4The room temperature hysteresis curve of nanoparticle sample, characterizes collection of illustrative plates, sees Fig. 8 accordingly.
Claims (3)
- A kind of 1. MnFe2O4The preparation method of nano magnetic material, it is characterised in that：According to manganese：Ferro element mol ratio is 1：2 claim Manganous salt sample, trivalent iron salt sample are taken, manganous salt sample will be weighed, trivalent iron salt sample is put into flask, and is being burnt After oleyl amine and each 40ml formation mixed liquor of oleic acid are then added into flask, then entered as solvent using 400ml benzyl ether in bottle Row heating, prepare three degree of symmetrical structures, four degree of symmetrical, six degree of symmetrical, MnFe of rhombic symmetry2O4Nano magnetic material；Three degree of symmetrical MnFe are prepared2O4Nano magnetic material, heating stepses are as follows：（a1）, first mixed liquor in flask is heated to 30 DEG C and the min of magnetic agitation 30；（b1）And then constant temperature 15min after mixed liquor in flask is heated into 120 DEG C；（c1）, mixed liquor in flask is then heated to 200 DEG C after constant temperature 2h；（d1）, mixed liquor in flask is finally heated to 290 DEG C after the h of constant temperature 1；Whole heating process is in N2Carried out under atmosphere protection, room temperature is naturally cooled to after the completion of heating, it is clear then to add suitable alcohols Wash and obtain three degree of symmetrical MnFe in microstructure after solution is thoroughly limpid, dries2O4Nano magnetic material, it is named as MFO120；Four degree of symmetrical MnFe are prepared2O4Nano magnetic material, heating stepses are as follows：（a2）, first mixed liquor in flask is heated to 30 DEG C and the min of magnetic agitation 30；（b2）And then by mixed liquor in flask be heated to 140 DEG C or 150 DEG C or 170 DEG C be cooled to 120 DEG C again after constant temperature 15min；（c2）, mixed liquor in flask is then heated to 200 DEG C after constant temperature 2h；（d2）, mixed liquor in flask is finally heated to 290 DEG C after the h of constant temperature 1；Whole heating process is in N2Carried out under atmosphere protection, room temperature is naturally cooled to after the completion of heating, it is clear then to add suitable alcohols Wash and obtain four degree of symmetrical MnFe in microstructure after solution is thoroughly limpid, dries2O4Nano magnetic material, it is named as MFO140, either MFO150 or MFO170；Six degree of symmetrical MnFe are prepared2O4Nano magnetic material, heating stepses are as follows：（a3）, first mixed liquor in flask is heated to 30 DEG C and the min of magnetic agitation 30；（b3）And then by mixed liquor in flask be heated to 160 DEG C be cooled to 120 DEG C again after constant temperature 15min；（c3）, mixed liquor in flask is then heated to 200 DEG C after constant temperature 2h；（d3）, mixed liquor in flask is finally heated to 290 DEG C after the h of constant temperature 1；Whole heating process is in N2Carried out under atmosphere protection, room temperature is naturally cooled to after the completion of heating, it is clear then to add suitable alcohols Wash and obtain six degree of symmetrical MnFe in microstructure after solution is thoroughly limpid, dries2O4Nano magnetic material, it is named as MFO160；The MnFe of rhombic symmetry is prepared2O4Nano magnetic material, heating stepses are as follows：（a4）, first mixed liquor in flask is heated to 30 DEG C and the min of magnetic agitation 30；（b4）And then by mixed liquor in flask be heated to 200 DEG C be cooled to 120 DEG C again after constant temperature 15min；（c4）, mixed liquor in flask is then heated to 200 DEG C after constant temperature 2h；（d4）, mixed liquor in flask is finally heated to 290 DEG C after the h of constant temperature 1；Whole heating process is in N2Carried out under atmosphere protection, room temperature is naturally cooled to after the completion of heating, it is clear then to add suitable alcohols Wash after solution is thoroughly limpid, dries and obtain the MnFe of rhombic symmetry in microstructure2O4Nano magnetic material, it is named as MFO200。
- A kind of 2. MnFe according to claim 12O4The preparation method of nano magnetic material, it is characterised in that：The divalence Manganese salt is divalence manganese acetylacetonate.
- A kind of 3. MnFe according to claim 12O4The preparation method of nano magnetic material, it is characterised in that：The trivalent Molysite is trivalent ferric acetyl acetonade.
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| 热分解法制备 MnFe2O4 纳米粒子及其超顺磁性;尤娜等;《物理实验》;20110228;第31卷(第2期);第11-14页 * |
| 硬磁ＣｏＦｅ２Ｏ４软磁ＣｏＦｅ２复合物的磁性研究;马永青等;《安徽大学学报(自然科学版)》;20150925;第40卷(第1期);第37-41页 * |
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