CN103833349A - La0.1Bi0.9FeO3/NiFe2O4 magnetoelectric composite powder and preparation method thereof - Google Patents
La0.1Bi0.9FeO3/NiFe2O4 magnetoelectric composite powder and preparation method thereof Download PDFInfo
- Publication number
- CN103833349A CN103833349A CN201410001123.7A CN201410001123A CN103833349A CN 103833349 A CN103833349 A CN 103833349A CN 201410001123 A CN201410001123 A CN 201410001123A CN 103833349 A CN103833349 A CN 103833349A
- Authority
- CN
- China
- Prior art keywords
- feo
- nife
- composite granule
- preparation
- sol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Magnetic Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention provides a La0.1Bi0.9FeO3/NiFe2O4 magnetoelectric composite powder and a preparation method thereof. The preparation method comprises the following steps: adding analytically pure Fe(NO3)3.9H2O, Bi(NO3)3.9H2O, La(NO3)3.6H2O and Ni(NO3)2.6H2O into distilled water to prepare a solution according to the general chemical formula xLa0.1Bi0.9FeO3/(1-x)NiFe2O4, wherein x is the mass percentage of La0.1Bi0.9FeO3 and is no less than 0.6 and no more than 0.9; adding citric acid into the solution, carrying out stirring to realize uniform mixing and adjusting a pH value so as to obtain a uniform sol B; and drying and calcining the sol B. The method can rapidly prepare the La0.1Bi0.9FeO3/NiFe2O4 magnetoelectric composite powder at a low temperature and has the advantages of simple process and conservation of energy; and the prepared magnetoelectric magnetic composite powder has good uniformity.
Description
Technical field
The invention belongs to material science, be specifically related to a kind of La
0.1bi
0.9feO
3/ NiFe
2o
4magnetoelectricity composite granule and preparation method thereof.
Background technology
Along with further developing of scientific and technical progress and technology of Internet of things, more and more higher to device microminiaturization, integrated requirement, the material of single performance is difficult to meet the requirement of modernization functional device, in order to develop the new device that can realize several functions simultaneously, this just needs development to have the type material of two or more function simultaneously, can realize the new device of several functions with development simultaneously, multi-iron material be exactly wherein one typically represent material.Multi-iron material is that one has ferroelectricity, ferromegnetism or ferroelastic material simultaneously, and there is the magnetoelectric effect that polarization and magnetized interaction produce, a kind of ferroelectric material and ferromagnetic material advantage type material of having concurrently, designing and researching and developing novel high-density memory device, spin electric device, the aspects such as magneto-electric coupled senser element all have wide practical use.
For example be expected to realize autotelegraph magnetic reader part fast, in order to substitute conventional iron electrical storage and magnetic memory device, this need to apply the problem in large local magnetic field can be avoided problem that ferroelectric memory reading of data exists or magneticstorage data writing time.In addition, due to ferroelectricity and ferromagnetic coexisting, make this material there is high specific inductivity and magnetic permeability simultaneously, can make high capacitance and large inductor integrated electronic devices and components, for the mutual interference problem that reduces number of devices, solution perceptual device and capacitive device on high density circuit board provides new thinking.Present ABO
3the BiFeO of type titanium ore structure
3it is a kind of typical single phase multi-iron material.Than other single phase multi-iron material BiFeO
3material has high Ne&1&el temperature (T
nbe about 370 ℃), in lower than this temperature range, there is G type antiferromagnetism (or weak ferromagnetism); Meanwhile, BiFeO
3there is high Curie temperature (T
cbe about 830 ℃), Theoretical Calculation shows to have large spontaneous polarization strength under room temperature, can substitute in many aspects the leaded ferroelectric material PbTiO of current application
3, have broad application prospects at aspects such as non-volatile ferroelectric memory or high-temperature electronic devices.High Curie temperature and Ne&1&el temperature make BiFeO
3become minority and at room temperature there is one of ferroelectricity and ferromagnetic multi-iron material simultaneously.Especially in recent years, BiFeO
3material causes the interest that people study gradually.
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) due to 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.At present the research of bismuth ferrite is mainly concentrated on by doping and compound to improving its multi-ferrum property aspect, doping mainly contains the doping of A position and the doping of B position.For example La doping causes BiFeO
3lattice parameter change and then make BiFeO
3ferroelectric properties and magnetic also obtained enhancing; Compound main introducing other mutually and then improve its ferroelectricity and magnetic.Conventionally the method for preparing magnetic composite powder 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, a kind of La is provided
0.1bi
0.9feO
3/ NiFe
2o
4magnetoelectricity composite granule and preparation method thereof, its preparation temperature is lower, method is simple, the La making
0.1bi
0.9feO
3/ NiFe
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/ NiFe
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) NiFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Ni (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, nickel 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 800-900 ℃, calcine 1-4h and obtain La
0.1bi
0.9feO
3/ NiFe
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/ NiFe
2o
4magnetoelectricity composite granule, this La
0.1bi
0.9feO
3/ NiFe
2o
4the chemical general formula of magnetoelectricity composite granule is xLa
0.1bi
0.9feO
3/ (1-x) NiFe
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, Ni (NO
3)
26H
2o and citric acid are raw material, and through adjust pH, dry, at 800-900 ℃, calcining obtains La
0.1bi
0.9feO
3/ NiFe
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/ NiFe
2o
4magnetoelectricity composite granule homogeneity is better, along with NiFe in composite granule
2o
4content increases, and saturation magnetization is increased to 15.2emu/g by 3.4emu/g, and coercive field is increased to 84.46 oersteds by 54.39 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%, NiFe
2o
4the XRD figure of composite granule under 800 ℃ of calcinings when mass percent is 10%.
Fig. 2 is for working as La
0.1bi
0.9feO
3mass percent be 80%, NiFe
2o
4the XRD figure of composite granule under 800 ℃ of calcinings when mass percent is 20%.
Fig. 3 is for working as La
0.1bi
0.9feO
3mass percent be 70%, NiFe
2o
4the XRD figure of composite granule under 800 ℃ of calcinings when mass percent is 30%.
Fig. 4 is for working as La
0.1bi
0.9feO
3mass percent be 60%, NiFe
2o
4the XRD figure of composite granule under 800 ℃ of calcinings when mass percent is 40%.
Fig. 5 is for working as La
0.1bi
0.9feO
3mass percent be 90%, NiFe
2o
4the SEM of composite granule powder after 800 ℃ of calcinings figure when mass percent is 10%.
Fig. 6 is for working as La
0.1bi
0.9feO
3mass percent be 80%, NiFe
2o
4the SEM of composite granule powder after 800 ℃ of calcinings figure when mass percent is 20%.
Fig. 7 is for working as La
0.1bi
0.9feO
3mass percent be 70%, NiFe
2o
4the SEM of composite granule powder after 800 ℃ of calcinings figure when mass percent is 30%.
Fig. 8 is for working as La
0.1bi
0.9feO
3mass percent be 60%, NiFe
2o
4the SEM of composite granule powder after 800 ℃ of calcinings figure when mass percent is 40%.
Fig. 9 is for working as La
0.1bi
0.9feO
3mass ratio is 90%, NiFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powder after 800 ℃ of calcinings while being 10%.
Figure 10 is for working as La
0.1bi
0.9feO
3mass ratio is 80%, NiFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powder after 800 ℃ of calcinings while being 20%.
Figure 11 is for working as La
0.1bi
0.9feO
3mass ratio is 70%, NiFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powder after 800 ℃ of calcinings while being 30%.
Figure 12 is for working as La
0.1bi
0.9feO
3mass ratio is 60%, NiFe
2o
4the magnetic hysteresis loop of mass ratio composite granule powder after 800 ℃ of calcinings while being 40%.
Embodiment
Below in conjunction with drawings and Examples, the present invention is elaborated.
1) press chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) NiFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Ni (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, nickel 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 800 ℃, calcines 1h and obtain La
0.1bi
0.9feO
3/ NiFe
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) NiFe
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 NiFe
2o
4.
As can be seen from Figure 5, 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, NiFe
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/ NiFe
2o
4the magnetic hysteresis loop of magnetoelectricity composite granule is comparatively level and smooth, and saturation magnetization is 3.4emu/g, and coercive field is 80.29 oersteds.
1) press chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) NiFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Ni (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, nickel 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 800 ℃, calcines 4h and obtain La
0.1bi
0.9feO
3/ NiFe
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) NiFe
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 NiFe
2o
4.
As can be seen from Figure 6, 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, NiFe
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/ NiFe
2o
4the magnetic hysteresis loop of magnetoelectricity composite granule is comparatively level and smooth, and saturation magnetization is 7.0emu/g, and coercive field is 54.37 oersteds.
1) press chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) NiFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Ni (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, nickel 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 800 ℃, calcines 2h and obtain La
0.1bi
0.9feO
3/ NiFe
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) NiFe
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 NiFe
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, NiFe
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/ NiFe
2o
4the magnetic hysteresis loop of magnetoelectricity composite granule is comparatively level and smooth, and saturation magnetization is 10.5emu/g, and coercive field is 76.12 oersteds.
1) press chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) NiFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Ni (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, nickel 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 800 ℃, calcines 3h and obtain La
0.1bi
0.9feO
3/ NiFe
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) NiFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.6.
As can be seen from Figure 4, 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 NiFe
2o
4.
As can be seen from Figure 8, 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, NiFe
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/ NiFe
2o
4the magnetic hysteresis loop of magnetoelectricity composite granule is comparatively level and smooth, and saturation magnetization is 15.2emu/g, and coercive field is 84.46 oersteds.
1) press chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) NiFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Ni (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, nickel 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 900 ℃, calcines 1h and obtain La
0.1bi
0.9feO
3/ NiFe
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) NiFe
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) NiFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Ni (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 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, nickel 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 820 ℃, calcines 4h and obtain La
0.1bi
0.9feO
3/ NiFe
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) NiFe
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) NiFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Ni (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, nickel 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 850 ℃, calcines 3h and obtain La
0.1bi
0.9feO
3/ NiFe
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) NiFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and x=0.7.
1) press chemical general formula xLa
0.1bi
0.9feO
3/ (1-x) NiFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Ni (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, nickel 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 870 ℃, calcines 2h and obtain La
0.1bi
0.9feO
3/ NiFe
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)/NiFe
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/ NiFe
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) NiFe
2o
4, by analytically pure Fe (NO
3)
39H
2o, Bi (NO
3)
39H
2o, La (NO
3)
36H
2o and Ni (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, nickel 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 800-900 ℃, calcine 1-4h and obtain La
0.1bi
0.9feO
3/ NiFe
2o
4magnetoelectricity composite granule.
2. a kind of La according to claim 1
0.1bi
0.9feO
3/ NiFe
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/ NiFe
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/ NiFe
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/ NiFe
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/ NiFe
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/ NiFe
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/ NiFe
2o
4magnetoelectricity composite granule, is characterized in that, this La
0.1bi
0.9feO
3/ NiFe
2o
4the chemical general formula of magnetoelectricity composite granule is xLa
0.1bi
0.9feO
3/ (1-x) NiFe
2o
4, wherein, x is La
0.1bi
0.9feO
3mass percent, and 0.6≤x≤0.9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410001123.7A CN103833349A (en) | 2014-01-02 | 2014-01-02 | La0.1Bi0.9FeO3/NiFe2O4 magnetoelectric composite powder and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410001123.7A CN103833349A (en) | 2014-01-02 | 2014-01-02 | La0.1Bi0.9FeO3/NiFe2O4 magnetoelectric composite powder and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103833349A true CN103833349A (en) | 2014-06-04 |
Family
ID=50797294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410001123.7A Pending CN103833349A (en) | 2014-01-02 | 2014-01-02 | La0.1Bi0.9FeO3/NiFe2O4 magnetoelectric composite powder and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103833349A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445996A (en) * | 2014-12-11 | 2015-03-25 | 陕西科技大学 | Multiferroic Bi0.96-xSr0.04RExFe0.94Mn0.04Cr0.02O3-NiFe2O4 composite film and preparation method thereof |
| CN106007695A (en) * | 2016-04-26 | 2016-10-12 | 北京工业大学 | Method for one-time synthesis of NFO-PZT-BFO composite multiferroic material by using precursor hydrothermal treatment |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2014
- 2014-01-02 CN CN201410001123.7A patent/CN103833349A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (2)
| Title |
|---|
| S. Y. WANG ET AL.: ""Electrical reliability and leakage mechanisms in highly resistive multiferroic La0.1Bi0.9FeO3 ceramics"", 《APPLIED PHYSICS LETTERS》, vol. 98, 13 April 2011 (2011-04-13), pages 152902 * |
| XIANMING LIU ET AL.: ""Synthesis and Characterization of Multiferroic NiFe2O4/BiFeO3 Nanocomposites by Modified Pechini Method"", 《ADVANCED MATERIALS RESEARCH》, vol. 197198, 21 February 2011 (2011-02-21), pages 456 - 459 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104445996A (en) * | 2014-12-11 | 2015-03-25 | 陕西科技大学 | Multiferroic Bi0.96-xSr0.04RExFe0.94Mn0.04Cr0.02O3-NiFe2O4 composite film and preparation method thereof |
| CN106007695A (en) * | 2016-04-26 | 2016-10-12 | 北京工业大学 | Method for one-time synthesis of NFO-PZT-BFO composite multiferroic material by using precursor hydrothermal treatment |
| CN106007695B (en) * | 2016-04-26 | 2018-08-28 | 北京工业大学 | It is a kind of to utilize the disposable synthetic method of the compound multi-iron materials of presoma hydro-thermal process NFO-PZT-BFO |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Kuruva et al. | Effect of Ni–Zr codoping on dielectric and magnetic properties of SrFe12O19 via sol–gel route | |
| CN103771846B (en) | BaFe12O19/Y3Fe5O12 two-phase magnetic composite powder and preparation method thereof | |
| Wu et al. | Preparation and magnetic properties of RFeO 3 nanocrystalline powders | |
| CN111196721A (en) | La1-xBixFeO3Rare earth ferrite magnetic material and preparation method thereof | |
| CN103833341A (en) | BaFe12O19/CoFe2O4 dual-phase magnetic composite powder and preparation method thereof | |
| Liu et al. | Influence of Co doping on the magnetic properties of Bi 2 Fe 4 O 9 powders | |
| Sharma et al. | Synthesis, structural, optical, electrical and Mössbauer spectroscopic studies of Co substituted Li0. 5Fe2. 5O4 | |
| CN103771847B (en) | La0.1Bi0.9FeO3/BiY2Fe5O12 magnetoelectric composite powder and preparation method thereof | |
| CN104557009A (en) | CoFe2O4-based nano-magnetic composite powder and preparation method thereof | |
| CN103771848B (en) | La0.1Bi0.9FeO3/CoFe2O4 magneto-electricity compound powder body and preparation method thereof | |
| CN102173763A (en) | Bismuth ferrititanate multiferroic material and sol-gel preparation method thereof | |
| Nath et al. | Magnetization and magnetic behavior of Ni1-xCdxFe2O4 ferrites | |
| CN104591721B (en) | Single-phase multiferroic M-type lead ferrite ceramic material and preparation method thereof | |
| Trukhanov et al. | Magnetic properties of the nonstoichiometric Sr‐doped manganites | |
| CN103787420A (en) | Method for preparing SrFe12O19 magnetic nano powder by using microwave hydrothermal method | |
| CN103833349A (en) | La0.1Bi0.9FeO3/NiFe2O4 magnetoelectric composite powder and preparation method thereof | |
| CN104556997A (en) | NiFe2O4/Bi2Fe4O9 two-phase magnetic composite powder and preparation method thereof | |
| Jiang et al. | The structure and magnetic properties of Eu-doped B i F e O 3 prepared by a solid-phase sintering method | |
| CN108640158B (en) | Preparation method of high-purity hexagonal sheet barium ferrite | |
| CN105645944B (en) | A kind of Bi2Fe4O9/BaFe12O19Composite ceramics and preparation method thereof | |
| CN104446449A (en) | Preparation method of BIT-Fe multiferroic ferroelectric ceramic | |
| Yao et al. | Correlation of the chemical composition, phase content, structural characteristics and magnetic properties of the Bi-substituted M-type hexaferrites | |
| Min et al. | Room-temperature multiferroic properties of Co-doped KNbO3 ceramics | |
| CN104591294A (en) | Bismuth ferrite based two-phase magnetic composite powder and preparation method thereof | |
| CN101811861A (en) | Nano-crystalline MnZn ferrite material with high saturation induction density and high resistivity and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140604 |