CN103771848B - La0.1Bi0.9FeO3/CoFe2O4 magneto-electricity compound powder body and preparation method thereof - Google Patents
La0.1Bi0.9FeO3/CoFe2O4 magneto-electricity compound powder body and preparation method thereof Download PDFInfo
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- CN103771848B CN103771848B CN201410001797.7A CN201410001797A CN103771848B CN 103771848 B CN103771848 B CN 103771848B CN 201410001797 A CN201410001797 A CN 201410001797A CN 103771848 B CN103771848 B CN 103771848B
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Abstract
The invention relates to a La0.1Bi0.9FeO3/CoFe2O4 magneto-electricity compound powder body and a preparation method thereof. The preparation method comprises the steps: according to a chemical general formula xLa0.1Bi0.9FeO3/(1-x)CoFe2O4, adding analytical-grade Fe(NO3)3.9H2O, Bi(NO3)3.9H2O, La (NO3)3.6H2O and Co(NO3)2.6H2O in distilled water to prepare a solution, wherein x is a mass percent of the La0.1Bi0.9FeO3, and is not less than 0.6 and not more than 0.9; adding citric acid in the solution, uniformly stirring, adjusting the pH value to obtain a uniform sol B; and drying the sol B and calcining. The invention is a method for rapidly preparing the La0.1Bi0.9FeO3/CoFe2O4 magneto-electricity compound powder body at a lower temperature; and the method is simple in process and energy-saving; and the prepared magneto-electricity compound powder body is better in uniformity.
Description
Technical field
The invention belongs to material science, be specifically related to a kind of La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule and preparation method thereof.
Background technology
Multi-ferroic material is the very important advanced function material of a large class, the components and parts utilizing multi-ferroic material to make have the functions such as conversion, transmission, process information, stored energy, save energy, are widely used in the field such as the energy, telecommunications, automatically control, communication, household electrical appliance, biology, health care, light industry, ore dressing, physics mine locating, military project.Along with the develop rapidly of mobile communication and computer technology, require that various electronics becomes Highgrade integration, multifunction, miniaturization and response fast more, thus higher standard is proposed to material, require components and parts not only Large Copacity, miniaturization, high speed, and there is the feature of reliability, weather resistance, anti-vibration and low cost, this just needs development to have the type material of two or more function simultaneously, multi-ferroic material also becomes in recent years a new popular research field in the world thereupon, wherein has the BiFeO of perovskite structure
3become a kind of important materials of everybody research, because BiFeO
3that more than room temperature has ferroelectricity and anti-ferromagnetic sole material simultaneously, its ferroelectrie Curie temperature is TC=830 DEG C, and antiferromagnetic Neel temperature is TN=370 DEG C, and there is coupling between two kinds of ferrous, namely regulate electrical property by magnetic field, or control magnetic property with electric field.
Current BiFeO
3there are three outstanding problems: (1) easily volatilizees due to Bi, must consider the balance on kinetics and thermodynamics during synthesis simultaneously, be therefore difficult to the BiFeO obtaining pure phase
3.To BiFeO
3the control of growth technique and condition becomes the work that one has challenge; (2) leakage current causes more greatly ferroelectricity to be difficult to measure; (3) BiFeO
3special G type anti-ferromagnetic structure, makes the BiFeO of macro-size
3at room temperature show very weak antiferromagnetism, these seriously hinder BiFeO
3the development of practical application.Ball magnetoelectric material is now wanted to have coercive field large as far as possible, high saturation magnetization and high magneto-electric coupled coefficient etc. in the industrial production, in order to obtain there is high saturation and magnetic intensity and high coercitive magnetoelectric material, usual people's selection doping vario-property or carry out compound with different materials and realize this purpose.Such as Hard Magnetic/soft magnetism compound is made up of with soft magnetism mutually Hard Magnetic phase, has very strong exchange-coupling interaction between them.In reverse magnetization process, by the impact of hard magnetic layer magnetic moment, the distribution in the magnetic moment deflection direction in soft magnetosphere is continuous print, reversal magnetization field larger or from interface more away from local magnetic moment more close to outer field orientation, and when being less than spin-exchange-coupled critical magnetic field in magnetic field, magnetic moment reversibly rotates.For ABO
3type calcium is admired ore deposit ferroelectric material, and the replacement of A position ion and B position ion can realize its structural adjustment, and finally reaches the object BiFeO changing performance
3carry out magnetic property and electrical property that certain element doping can reduce leakage current and then improve bismuth ferrite; CoFe
2o
4there is high coercive field and saturation magnetization, CoFe
2o
4introducing can improve BiFeO
3magnetic property.
Usually the method preparing magnetoelectricity composite granule first adopts solid phase method to prepare each single-phase powder respectively, then carries out mechanically mixing.This method, the calcining temperature not only required for complex process is high, and the composite granule prepared in grain-size, carries out mixing cause homogeneity poor, finally directly has influence on the performance of composite granule.
Summary of the invention
The object of the invention is to overcome the problems of the prior art, La is provided
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule and preparation method thereof, its preparation temperature is lower, method simple, obtained La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule homogeneity is better.
For achieving the above object, the present invention adopts following technical scheme:
A kind of La
0.1bi
0.9feO
3/ CoFe
2o
4the preparation method of magnetoelectricity composite granule, comprises the following steps:
1) by chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Co (NO
3)
26H
2o joins in distilled water and is mixed with solution; Wherein, x is La
0.1bi
0.9feO
3mass percent, and 0.6≤x≤0.9;
2) in the solution of step 1), add citric acid, heat at 80-100 DEG C and stir, obtaining Sol A, wherein, the molar weight adding citric acid be iron ion in solution, bismuth ion, lanthanum ion, cobalt ion integral molar quantity 2-4 doubly;
3), under stirring, the pH value of Sol A is adjusted to 6.5-7.5, obtains uniform sol B;
4) sol B is dry at 180-200 DEG C, obtain chocolate and to loosen shape xerogel;
5), after xerogel being ground, at 700-800 DEG C, calcine 1-4h obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule.
Described step 2) in heating realized by heating in water bath.
Described step 2) in stir time be 1 ~ 2 hour.
In described step 3), pH value adopts quadrol or ammoniacal liquor to regulate.
Time dry in described step 4) is 2-4 hour.
In described step 4), drying is carried out in vacuum drying oven.
In described step 5), calcining is carried out in electric furnace.
A kind of La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule, is characterized in that, this La
0.1bi
0.9feO
3/ CoFe
2o
4the chemical general formula of magnetoelectricity composite granule is xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and 0.6≤x≤0.9.
Relative to prior art, the beneficial effect that the present invention has: the present invention is with Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o, Co (NO
3)
26H
2o and citric acid are raw material, and through adjust pH, drying, at 700-800 DEG C, calcining obtains La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule; Preparation temperature of the present invention is lower, method simple, and saves the energy; The La that the present invention obtains
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule homogeneity is better, along with CoFe in composite granule
2o
4content increases, saturation magnetization is increased to 26.1emu/g by 4.8emu/g, coercive field is increased to 1930.73 oersteds by 1260.14 oersteds, overcomes the existing problem preparing higher, the obtained composite granule poor-performing of synthesis temperature in the method for composite granule.
Accompanying drawing explanation
Fig. 1 is for work as La
0.1bi
0.9feO
3mass percent be 90%, CoFe
2o
4the XRD figure of composite granule under 700 DEG C of calcinings when mass percent is 10%.
Fig. 2 is for work as La
0.1bi
0.9feO
3mass percent be 80%, CoFe
2o
4the XRD figure of composite granule under 700 DEG C of calcinings when mass percent is 20%.
Fig. 3 is for work as La
0.1bi
0.9feO
3mass percent be 70%, CoFe
2o
4the XRD figure of composite granule under 700 DEG C of calcinings when mass percent is 30%.
Fig. 4 is for work as La
0.1bi
0.9feO
3mass percent be 60%, CoFe
2o
4the XRD figure of composite granule under 700 DEG C of calcinings when mass percent is 40%.
Fig. 5 is for work as La
0.1bi
0.9feO
3mass percent be 90%, CoFe
2o
4the SEM figure of composite granule powder after 700 DEG C of calcinings when mass percent is 10%.
Fig. 6 is for work as La
0.1bi
0.9feO
3mass percent be 80%, CoFe
2o
4the SEM figure of composite granule powder after 700 DEG C of calcinings when mass percent is 20%.
Fig. 7 is for work as La
0.1bi
0.9feO
3mass percent be 70%, CoFe
2o
4the SEM figure of composite granule powder after 700 DEG C of calcinings when mass percent is 30%.
Fig. 8 is for work as La
0.1bi
0.9feO
3mass percent be 60%, CoFe
2o
4the SEM figure of composite granule powder after 700 DEG C of calcinings when mass percent is 40%.
Fig. 9 is for work as La
0.1bi
0.9feO
3mass ratio is 90%, CoFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powders after 700 DEG C of calcinings when being 10%.
Figure 10 is for work as La
0.1bi
0.9feO
3mass ratio is 80%, CoFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powders after 700 DEG C of calcinings when being 20%.
Figure 11 is for work as La
0.1bi
0.9feO
3mass ratio is 70%, CoFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powders after 700 DEG C of calcinings when being 30%.
Figure 12 is for work as La
0.1bi
0.9feO
3mass ratio is 60%, CoFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powders after 700 DEG C of calcinings when being 40%.
Embodiment
Below in conjunction with drawings and Examples, the present invention is elaborated.
Embodiment 1
1) by chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Co (NO
3)
26H
2o joins in distilled water and is mixed with solution; Wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.9;
2) in the solution of step 1), add citric acid, under 80 DEG C of heating in water bath, stir 1h, obtain Sol A, wherein, the molar weight adding citric acid be iron ion in solution, bismuth ion, lanthanum ion, 2 times of cobalt ion four metal ion species integral molar quantity;
3), under stirring, adopt quadrol that the pH value of Sol A is adjusted to 6.5, obtain uniform sol B;
4) sol B is put into vacuum drying oven, dry 2h at 200 DEG C, obtain chocolate and to loosen shape xerogel;
5) load after xerogel grinding in crucible, and crucible is placed in electric furnace and at 700 DEG C, calcines 1h obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule.
The chemical general formula of the magnetoelectricity composite granule that the present embodiment obtains is xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.9.
As can be seen from Figure 1, have containing perovskite typed La in the magnetoelectricity composite granule that prepared by the present embodiment
0.1bi
0.9feO
3with spinel type CoFe
2o
4.
As can be seen from Figure 5, the La for preparing of the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4in magnetoelectricity composite granule, the distribution of two-phase crystal grain is comparatively even, and two-phase grain development is better, wherein La
0.1bi
0.9feO
3grain-size is about 200nm, CoFe
2o
4grain-size be less than 100nm.
As can be seen from Figure 9, the La for preparing of the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4the magnetic hysteresis loop of magnetoelectricity composite granule is comparatively level and smooth, and saturation magnetization is 4.8emu/g, and coercive field is 1411.39 oersteds.
Embodiment 2
1) by chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Co (NO
3)
26H
2o joins in distilled water and is mixed with solution; Wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.8;
2) in the solution of step 1), add citric acid, under 100 DEG C of heating in water bath, stir 1h, obtain Sol A, wherein, the molar weight adding citric acid be iron ion in solution, bismuth ion, lanthanum ion, 3 times of cobalt ion four metal ion species integral molar quantity;
3), under stirring, adopt quadrol that the pH value of Sol A is adjusted to 7.5, obtain uniform sol B;
4) sol B is put into vacuum drying oven, dry 3h at 190 DEG C, obtain chocolate and to loosen shape xerogel;
5) load after xerogel grinding in crucible, and crucible is placed in electric furnace and at 700 DEG C, calcines 4h obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule.
The chemical general formula of the magnetoelectricity composite granule that the present embodiment obtains is xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.8.
As can be seen from Figure 2, have containing perovskite typed La in the magnetoelectricity composite granule that prepared by the present embodiment
0.1bi
0.9feO
3with spinel type CoFe
2o
4.
As can be seen from Figure 6, the La for preparing of the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4in magnetoelectricity composite granule, the distribution of two-phase crystal grain is comparatively even, and two-phase grain development is better, wherein La
0.1bi
0.9feO
3grain-size is about 200nm, CoFe
2o
4grain-size be less than 100nm.
As can be seen from Figure 10, the La for preparing of the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4the magnetic hysteresis loop of magnetoelectricity composite granule is comparatively level and smooth, and saturation magnetization is 9.9emu/g, and coercive field is 1260.14 oersteds.
Embodiment 3
1) by chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Co (NO
3)
26H
2o joins in distilled water and is mixed with solution; Wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.7;
2) in the solution of step 1), add citric acid, under 90 DEG C of heating in water bath, stir 2h, obtain Sol A, wherein, the molar weight adding citric acid be iron ion in solution, bismuth ion, lanthanum ion, 4 times of cobalt ion four metal ion species integral molar quantity;
3), under stirring, adopt quadrol that the pH value of Sol A is adjusted to 7, obtain uniform sol B;
4) sol B is put into vacuum drying oven, dry 4h at 180 DEG C, obtain chocolate and to loosen shape xerogel;
5) load after xerogel grinding in crucible, and crucible is placed in electric furnace and at 700 DEG C, calcines 2h obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule.
The chemical general formula of the magnetoelectricity composite granule that the present embodiment obtains is xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.7.
As can be seen from Figure 3, have containing perovskite typed La in the magnetoelectricity composite granule that prepared by the present embodiment
0.1bi
0.9feO
3with spinel type CoFe
2o
4.
As can be seen from Figure 7, in magnetoelectricity composite granule prepared by the present embodiment, the distribution of two-phase crystal grain is comparatively even, and two-phase grain development is better, wherein La
0.1bi
0.9feO
3grain-size is about 200nm, CoFe
2o
4grain-size be less than 100nm.
As can be seen from Figure 11, the La for preparing of the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4the magnetic hysteresis loop of magnetoelectricity composite granule is comparatively level and smooth, and saturation magnetization is 16.8emu/ gram, and coercive field is 1485.92 oersteds.
Embodiment 4
1) by chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Co (NO
3)
26H
2o joins in distilled water and is mixed with solution; Wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.6;
2) in the solution of step 1), add citric acid, under 85 DEG C of heating in water bath, stir 1.5h, obtain Sol A, wherein, the molar weight adding citric acid be iron ion in solution, bismuth ion, lanthanum ion, 3 times of cobalt ion four metal ion species integral molar quantity;
3), under stirring, adopt quadrol that the pH value of Sol A is adjusted to 6.5, obtain uniform sol B;
4) sol B is put into vacuum drying oven, dry 2h at 195 DEG C, obtain chocolate and to loosen shape xerogel;
5) load after xerogel grinding in crucible, and crucible is placed in electric furnace and at 700 DEG C, calcines 3h obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule.
The chemical general formula of the magnetoelectricity composite granule that the present embodiment obtains is xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.6.
As can be seen from Figure 4, the La for preparing of the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4have containing perovskite typed La in magnetoelectricity composite granule
0.1bi
0.9feO
3with spinel type CoFe
2o
4.
As can be seen from Figure 8, the La for preparing of the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4in magnetoelectricity composite granule, the distribution of two-phase crystal grain is comparatively even, and two-phase grain development is better, wherein La
0.1bi
0.9feO
3grain-size is about 200nm, CoFe
2o
4grain-size be less than 100nm.
As can be seen from Figure 12, the La for preparing of the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4the magnetic hysteresis loop of magnetoelectricity composite granule is comparatively level and smooth, and saturation magnetization is 22.6emu/ gram, and coercive field is 1930.73 oersteds.
Embodiment 5
1) by chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Co (NO
3)
26H
2o joins in distilled water and is mixed with solution; Wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.9;
2) in the solution of step 1), add citric acid, under 100 DEG C of heating in water bath, stir 1h, obtain Sol A, wherein, the molar weight adding citric acid be iron ion in solution, bismuth ion, lanthanum ion, 2 times of cobalt ion four metal ion species integral molar quantity;
3), under stirring, adopt ammoniacal liquor that the pH value of Sol A is adjusted to 6.5, obtain uniform sol B;
4) sol B is put into vacuum drying oven, dry 4h at 180 DEG C, obtain chocolate and to loosen shape xerogel;
5) load after xerogel grinding in crucible, and crucible is placed in electric furnace and at 800 DEG C, calcines 1h obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule.
The chemical general formula of the magnetoelectricity composite granule that the present embodiment obtains is xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.9.
Embodiment 6
1) by chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, by analytically pure Fe (NO
3)
3.9H
2o, Bi (NO
3)
3.9H
2o, La (NO
3)
3.6H
2o and Co (NO
3)
2.6H
2o joins in distilled water and is mixed with solution; Wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.8;
2) in the solution of step 1), add citric acid, under 95 DEG C of heating in water bath, stir 1.5h, obtain Sol A, wherein, the molar weight adding citric acid be iron ion in solution, bismuth ion, lanthanum ion, 3 times of cobalt ion four metal ion species integral molar quantity;
3), under stirring, adopt ammoniacal liquor that the pH value of Sol A is adjusted to 7.5, obtain uniform sol B;
4) sol B is put into vacuum drying oven, dry 3h at 185 DEG C, obtain chocolate and to loosen shape xerogel;
5) load after xerogel grinding in crucible, and crucible is placed in electric furnace and at 720 DEG C, calcines 4h obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule.
The chemical general formula of the magnetoelectricity composite granule that the present embodiment obtains is xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.8.
Embodiment 7
1) by chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Co (NO
3)
26H
2o joins in distilled water and is mixed with solution; Wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.7;
2) in the solution of step 1), add citric acid, under 87 DEG C of heating in water bath, stir 1.5h, obtain Sol A, wherein, the molar weight adding citric acid be iron ion in solution, bismuth ion, lanthanum ion, 4 times of cobalt ion four metal ion species integral molar quantity;
3), under stirring, adopt ammoniacal liquor that the pH value of Sol A is adjusted to 7, obtain uniform sol B;
4) sol B is put into vacuum drying oven, dry 2h at 190 DEG C, obtain chocolate and to loosen shape xerogel;
5) load after xerogel grinding in crucible, and crucible is placed in electric furnace and at 750 DEG C, calcines 3h obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule.
The chemical general formula of the magnetoelectricity composite granule that the present embodiment obtains is xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.7.
Embodiment 8
1) by chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Co (NO
3)
26H
2o joins in distilled water and is mixed with solution; Wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.6;
2) in the solution of step 1), add citric acid, under 80 DEG C of heating in water bath, stir 2h, obtain Sol A, wherein, the molar weight adding citric acid be iron ion in solution, bismuth ion, lanthanum ion, 3 times of cobalt ion four metal ion species integral molar quantity;
3), under stirring, adopt ammoniacal liquor that the pH value of Sol A is adjusted to 6.5, obtain uniform sol B;
4) sol B is put into vacuum drying oven, dry 2h at 200 DEG C, obtain chocolate and to loosen shape xerogel;
5) load after xerogel grinding in crucible, and crucible is placed in electric furnace and at 770 DEG C, calcines 2h obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule.
The chemical general formula of the magnetoelectricity composite granule that the present embodiment obtains is xLa
0.1bi
0.9feO
3/ (1-x)/CoFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.6.
Claims (7)
1. a La
0.1bi
0.9feO
3/ CoFe
2o
4the preparation method of magnetoelectricity composite granule, is characterized in that, comprises the following steps:
1) by chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Co (NO
3)
26H
2o joins in distilled water and is mixed with solution; Wherein, x is La
0.1bi
0.9feO
3mass percent, and 0.6≤x≤0.9;
2) to step 1) solution in add citric acid, heat at 80-100 DEG C and stir, obtaining Sol A, wherein, the molar weight adding citric acid be iron ion in solution, bismuth ion, lanthanum ion, cobalt ion integral molar quantity 2-4 doubly;
3), under stirring, the pH value of Sol A is adjusted to 6.5-7.5, obtains uniform sol B;
4) sol B is dry at 180-200 DEG C, obtain chocolate and to loosen shape xerogel;
5), after xerogel being ground, at 700-800 DEG C, calcine 1-4h obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule;
Described step 3) in pH value be adopt quadrol regulate.
2. a kind of La according to claim 1
0.1bi
0.9feO
3/ CoFe
2o
4the preparation method of magnetoelectricity composite granule, is characterized in that, described step 2) in heating realized by heating in water bath.
3. a kind of La according to claim 1
0.1bi
0.9feO
3/ CoFe
2o
4the preparation method of magnetoelectricity composite granule, is characterized in that, described step 2) in stir time be 1 ~ 2 hour.
4. a kind of La according to claim 1
0.1bi
0.9feO
3/ CoFe
2o
4the preparation method of magnetoelectricity composite granule, is characterized in that, described step 4) in the dry time be 2-4 hour.
5. a kind of La according to claim 1
0.1bi
0.9feO
3/ CoFe
2o
4the preparation method of magnetoelectricity composite granule, is characterized in that, described step 4) in drying carry out in vacuum drying oven.
6. a kind of La according to claim 1
0.1bi
0.9feO
3/ CoFe
2o
4the preparation method of magnetoelectricity composite granule, is characterized in that, described step 5) in calcining carry out in electric furnace.
7. the La for preparing of method as claimed in claim 1
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule, is characterized in that, this La
0.1bi
0.9feO
3/ CoFe
2o
4the chemical general formula of magnetoelectricity composite granule is xLa
0.1bi
0.9feO
3/ (1-x) CoFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and 0.6≤x≤0.9.
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| CN102086119A (en) * | 2010-12-09 | 2011-06-08 | 华中科技大学 | Method for preparing room-temperature multiferroic BiFeO3-SrTiO3 sosoloid ceramics |
| CN102503391A (en) * | 2011-10-20 | 2012-06-20 | 陕西科技大学 | Preparation method of bismuth ferrite-based composite material with high ferromagnetic and ferroelectric properties |
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| CN102086119A (en) * | 2010-12-09 | 2011-06-08 | 华中科技大学 | Method for preparing room-temperature multiferroic BiFeO3-SrTiO3 sosoloid ceramics |
| CN102503391A (en) * | 2011-10-20 | 2012-06-20 | 陕西科技大学 | Preparation method of bismuth ferrite-based composite material with high ferromagnetic and ferroelectric properties |
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| Title |
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| 娄本浊等.(1-x)BiFeO3-xCoFe2O4复合陶瓷介电性能的研究.《压电与声光》.2012,第34卷(第1期),129-132. * |
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