CN103771848A - 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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- CN103771848A CN103771848A CN201410001797.7A CN201410001797A CN103771848A CN 103771848 A CN103771848 A CN 103771848A CN 201410001797 A CN201410001797 A CN 201410001797A CN 103771848 A CN103771848 A CN 103771848A
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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, utilize the components and parts that multi-ferroic material is made to there is the functions such as conversion, transmission, process information, stored energy, save energy, be widely used in the fields such as the energy, telecommunications, control automatically, 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 various electronicss to become Highgrade integration, multifunction, miniaturization and quick responseization more, thereby material is proposed to higher standard, require not only large capacity, miniaturization, high-speed of components and parts, and there is reliability, weather resistance, anti-vibration and feature cheaply, 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 room temperature has ferroelectricity and anti-ferromagnetic unique material above simultaneously, its ferroelectrie Curie temperature is TC=830 ℃, and antiferromagnetic Neel temperature is TN=370 ℃, and has coupling between two kinds of iron, regulate electrical property by magnetic field, or control magnetic property with electric field.
BiFeO at present
3there are three outstanding problems: (1), because Bi easily volatilizees, must consider the balance on kinetics and thermodynamics when synthetic simultaneously, is therefore difficult to obtain the BiFeO of pure phase
3.To BiFeO
3the control of growth technique and condition becomes a job with 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 have seriously hindered BiFeO
3the development of practical application.In industrial production, want now ball magnetoelectric material to there is large as far as possible coercive field, high saturation magnetization and high magneto-electric coupled coefficient etc., in order to obtain having high saturation and magnetic intensity and high coercitive magnetoelectric material, conventionally people select to carry out the compound this purpose that realizes with doping vario-property or with different materials.For example Hard Magnetic/soft magnetism is compound to be made up of with soft magnetism mutually Hard Magnetic phase, has very strong exchange-coupling interaction between them.In reverse magnetization process, be subject to the impact of hard magnetic layer magnetic moment, the distribution of the magnetic moment deflection direction in soft magnetosphere is continuous, and reversal magnetization field is larger or the local magnetic moment away from more approaches outer field orientation from interface, and magnetic moment can reversibly rotate while being less than spin-exchange-coupled critical magnetic field in magnetic field.For ABO
3the type calcium ore deposit ferroelectric material of admiring, the replacement of A position ion and B position ion can realize its structural adjustment, and finally reaches the object BiFeO that changes 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.
Conventionally the method for preparing magnetoelectricity composite granule is first to adopt solid phase method to prepare respectively each single-phase powder, then carries out mechanically mixing.This method, not only the needed calcining temperature of complex process is high, and the composite granule of preparing is in grain-size, to mix to 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 is simple, the La making
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) press 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 and in distilled water, 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 and stir at 80-100 ℃, obtain Sol A, wherein, the molar weight that adds citric acid is iron ion in solution, bismuth ion, lanthanum ion, cobalt ion integral molar quantity 2-4 times;
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 ℃, obtain the loose shape xerogel of chocolate;
5) after xerogel is ground, at 700-800 ℃, calcine 1-4h and obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule.
Described step 2) in heating realize by heating in water bath.
Described step 2) in stir time be 1～2 hour.
In described step 3), pH value is to adopt quadrol or ammoniacal liquor to regulate.
In described step 4), the dry time is 2-4 hour.
In described step 4), be dried and carry 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.
With respect 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, dry, at 700-800 ℃, calcining obtains La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule; Preparation temperature of the present invention is lower, method is simple, and saves the energy; The La that the present invention makes
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, has overcome that synthesis temperature in the existing method of preparing composite granule is higher, the problem of the composite granule poor-performing that makes.
Accompanying drawing explanation
Fig. 1 is for working as La
0.1bi
0.9feO
3mass percent be 90%, CoFe
2o
4the XRD figure of composite granule under 700 ℃ of calcinings when mass percent is 10%.
Fig. 2 is for working as La
0.1bi
0.9feO
3mass percent be 80%, CoFe
2o
4the XRD figure of composite granule under 700 ℃ of calcinings when mass percent is 20%.
Fig. 3 is for working as La
0.1bi
0.9feO
3mass percent be 70%, CoFe
2o
4the XRD figure of composite granule under 700 ℃ of calcinings when mass percent is 30%.
Fig. 4 is for working as La
0.1bi
0.9feO
3mass percent be 60%, CoFe
2o
4the XRD figure of composite granule under 700 ℃ of calcinings when mass percent is 40%.
Fig. 5 is for working as La
0.1bi
0.9feO
3mass percent be 90%, CoFe
2o
4the SEM of composite granule powder after 700 ℃ of calcinings figure when mass percent is 10%.
Fig. 6 is for working as La
0.1bi
0.9feO
3mass percent be 80%, CoFe
2o
4the SEM of composite granule powder after 700 ℃ of calcinings figure when mass percent is 20%.
Fig. 7 is for working as La
0.1bi
0.9feO
3mass percent be 70%, CoFe
2o
4the SEM of composite granule powder after 700 ℃ of calcinings figure when mass percent is 30%.
Fig. 8 is for working as La
0.1bi
0.9feO
3mass percent be 60%, CoFe
2o
4the SEM of composite granule powder after 700 ℃ of calcinings figure when mass percent is 40%.
Fig. 9 is for working as La
0.1bi
0.9feO
3mass ratio is 90%, CoFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powder after 700 ℃ of calcinings while being 10%.
Figure 10 is for working as La
0.1bi
0.9feO
3mass ratio is 80%, CoFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powder after 700 ℃ of calcinings while being 20%.
Figure 11 is for working as La
0.1bi
0.9feO
3mass ratio is 70%, CoFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powder after 700 ℃ of calcinings while being 30%.
Figure 12 is for working as La
0.1bi
0.9feO
3mass ratio is 60%, CoFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powder after 700 ℃ of calcinings while being 40%.
Embodiment
Below in conjunction with drawings and Examples, the present invention is elaborated.
Embodiment 1
1) press 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 and in distilled water, 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 ℃ of heating in water bath, stir 1h, obtain Sol A, wherein, the molar weight that adds citric acid is iron ion in solution, bismuth ion, lanthanum ion, cobalt ion four metal ion species integral molar quantities 2 times;
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 ℃, obtains the loose shape xerogel of chocolate;
5) after will xerogel grinding, pack in crucible, and crucible is placed in to electric furnace at 700 ℃, calcines 1h and 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 makes 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, in the magnetoelectricity composite granule that prepared by the present embodiment, there is the perovskite typed of containing La
0.1bi
0.9feO
3with spinel type CoFe
2o
4.
As can be seen from Figure 5, the La that prepared by the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4in magnetoelectricity composite granule, two-phase crystal grain distributes comparatively evenly, and two-phase crystal grain grows better, wherein La
0.1bi
0.9feO
3grain-size is 200nm left and right, CoFe
2o
4grain-size be less than 100nm.
As can be seen from Figure 9, the La that prepared by 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.
1) press 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 and in distilled water, 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 ℃ of heating in water bath, stir 1h, obtain Sol A, wherein, the molar weight that adds citric acid is iron ion in solution, bismuth ion, lanthanum ion, cobalt ion four metal ion species integral molar quantities 3 times;
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 ℃, obtains the loose shape xerogel of chocolate;
5) after will xerogel grinding, pack in crucible, and crucible is placed in to electric furnace at 700 ℃, calcines 4h and 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 makes 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, in the magnetoelectricity composite granule that prepared by the present embodiment, there is the perovskite typed of containing La
0.1bi
0.9feO
3with spinel type CoFe
2o
4.
As can be seen from Figure 6, the La that prepared by the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4in magnetoelectricity composite granule, two-phase crystal grain distributes comparatively evenly, and two-phase crystal grain grows better, wherein La
0.1bi
0.9feO
3grain-size is 200nm left and right, CoFe
2o
4grain-size be less than 100nm.
As can be seen from Figure 10, the La that prepared by 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.
1) press 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 and in distilled water, 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 ℃ of heating in water bath, stir 2h, obtain Sol A, wherein, the molar weight that adds citric acid is iron ion in solution, bismuth ion, lanthanum ion, cobalt ion four metal ion species integral molar quantities 4 times;
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 ℃, obtains the loose shape xerogel of chocolate;
5) after will xerogel grinding, pack in crucible, and crucible is placed in to electric furnace at 700 ℃, calcines 2h and 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 makes 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, in the magnetoelectricity composite granule that prepared by the present embodiment, there is the perovskite typed of containing La
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, two-phase crystal grain distributes comparatively evenly, and two-phase crystal grain grows better, wherein La
0.1bi
0.9feO
3grain-size is 200nm left and right, CoFe
2o
4grain-size be less than 100nm.
As can be seen from Figure 11, the La that prepared by 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.
1) press 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 and in distilled water, 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 ℃ of heating in water bath, stir 1.5h, obtain Sol A, wherein, the molar weight that adds citric acid is iron ion in solution, bismuth ion, lanthanum ion, cobalt ion four metal ion species integral molar quantities 3 times;
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 ℃, obtains the loose shape xerogel of chocolate;
5) after will xerogel grinding, pack in crucible, and crucible is placed in to electric furnace at 700 ℃, calcines 3h and 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 makes 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 that prepared by the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4in magnetoelectricity composite granule, there is the perovskite typed of containing La
0.1bi
0.9feO
3with spinel type CoFe
2o
4.
As can be seen from Figure 8, the La that prepared by the present embodiment
0.1bi
0.9feO
3/ CoFe
2o
4in magnetoelectricity composite granule, two-phase crystal grain distributes comparatively evenly, and two-phase crystal grain grows better, wherein La
0.1bi
0.9feO
3grain-size is 200nm left and right, CoFe
2o
4grain-size be less than 100nm.
As can be seen from Figure 12, the La that prepared by 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.
1) press 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 and in distilled water, 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 ℃ of heating in water bath, stir 1h, obtain Sol A, wherein, the molar weight that adds citric acid is iron ion in solution, bismuth ion, lanthanum ion, cobalt ion four metal ion species integral molar quantities 2 times;
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 ℃, obtains the loose shape xerogel of chocolate;
5) after will xerogel grinding, pack in crucible, and crucible is placed in to electric furnace at 800 ℃, calcines 1h and 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 makes 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.
1) press 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 and in distilled water, 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 ℃ of heating in water bath, stir 1.5h, obtain Sol A, wherein, the molar weight that adds citric acid is iron ion in solution, bismuth ion, lanthanum ion, cobalt ion four metal ion species integral molar quantities 3 times;
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 ℃, obtains the loose shape xerogel of chocolate;
5) after will xerogel grinding, pack in crucible, and crucible is placed in to electric furnace at 720 ℃, calcines 4h and 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 makes 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) press 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 and in distilled water, 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 ℃ of heating in water bath, stir 1.5h, obtain Sol A, wherein, the molar weight that adds citric acid is iron ion in solution, bismuth ion, lanthanum ion, cobalt ion four metal ion species integral molar quantities 4 times;
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 ℃, obtains the loose shape xerogel of chocolate;
5) after will xerogel grinding, pack in crucible, and crucible is placed in to electric furnace at 750 ℃, calcines 3h and 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 makes 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) press 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 and in distilled water, 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 ℃ of heating in water bath, stir 2h, obtain Sol A, wherein, the molar weight that adds citric acid is iron ion in solution, bismuth ion, lanthanum ion, cobalt ion four metal ion species integral molar quantities 3 times;
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 ℃, obtains the loose shape xerogel of chocolate;
5) after will xerogel grinding, pack in crucible, and crucible is placed in to electric furnace at 770 ℃, calcines 2h and 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 makes 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 (8)
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) press 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 and in distilled water, 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 and stir at 80-100 ℃, obtain Sol A, wherein, the molar weight that adds citric acid is iron ion in solution, bismuth ion, lanthanum ion, cobalt ion integral molar quantity 2-4 times;
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 ℃, obtain the loose shape xerogel of chocolate;
5) after xerogel is ground, at 700-800 ℃, calcine 1-4h and obtain La
0.1bi
0.9feO
3/ CoFe
2o
4magnetoelectricity composite granule.
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 realize 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, in described step 3), pH value is to adopt quadrol or ammoniacal liquor to regulate.
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, in described step 4), the dry time is 2-4 hour.
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, in described step 4), is dried and carries out in vacuum drying oven.
7. 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, in described step 5), calcining is carried out in electric furnace.
8. the La that method prepares 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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| CN105062478A (en) * | 2015-08-10 | 2015-11-18 | 中国科学院新疆理化技术研究所 | Biological method for preparing ferrite-bismuth ferrite composite fluorescent material |
| CN106745303A (en) * | 2017-02-27 | 2017-05-31 | 陕西科技大学 | A kind of three-dimensional flower ball-shaped cadmium ferrite bismuth meal body and preparation method thereof |
| CN108249392A (en) * | 2016-11-30 | 2018-07-06 | 连展科技电子（昆山）有限公司 | Mushroom granule, heat conduction material and method for producing mushroom granule |
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| 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 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105062478A (en) * | 2015-08-10 | 2015-11-18 | 中国科学院新疆理化技术研究所 | Biological method for preparing ferrite-bismuth ferrite composite fluorescent material |
| CN108249392A (en) * | 2016-11-30 | 2018-07-06 | 连展科技电子（昆山）有限公司 | Mushroom granule, heat conduction material and method for producing mushroom granule |
| CN108249392B (en) * | 2016-11-30 | 2021-02-09 | 连展科技电子（昆山）有限公司 | Mushroom granule, heat conduction material and method for producing mushroom granule |
| CN106745303A (en) * | 2017-02-27 | 2017-05-31 | 陕西科技大学 | A kind of three-dimensional flower ball-shaped cadmium ferrite bismuth meal body and preparation method thereof |
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