CN111087023A - Room temperature multiferroic material Ba4SmFe0.5Nb9.5O30Preparation method of (1) and prepared room-temperature multiferroic material - Google Patents
Room temperature multiferroic material Ba4SmFe0.5Nb9.5O30Preparation method of (1) and prepared room-temperature multiferroic material Download PDFInfo
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Abstract
The invention discloses a room-temperature multiferroic material Ba4SmFe0.5Nb9.5O30The prepared room temperature multiferroic material is weighed and BaCO is added3,Sm2O3,Fe2O3,Nb2O5The mixture is put into an agate mortar for grinding and is uniformly mixed; adding Al2O3Placing the crucible made of the material in a muffle furnace, heating to 1100 ℃, and preserving heat for 5 hours; cooling the calcined sample at a slow rate to room temperature; re-grinding, heating the sample subjected to secondary grinding to 1350 ℃ at the speed of 3 ℃/min, and preserving heat for 5 hours; cooling the sample to room temperature at the speed of 1 ℃/min after heat preservation to obtain Ba4SmFe0.5Nb9.5O30Room temperature multiferroic materials. The multiferroic material is crystallized into a tungsten bronze structure, a sample is flaky particles, and the coexistence characteristics of ferromagnetism and ferroelectricity are shown at room temperature. The invention has simple preparation process and low cost, and can realize large batchAnd (4) preparation and production.
Description
Technical Field
The invention belongs to the field of multiferroic material research, and particularly relates to a room-temperature multiferroic material Ba4SmFe0.5Nb9.5O30The preparation method and the prepared room temperature multiferroic material.
Background
The ferroic order includes ferroelasticity, ferromagnetism and ferroelectricity, and a material in which two or more ferroic orders exist simultaneously is called a multiferroic material, for example, a ferromagnetic/ferroelectric coexistent material called a magnetoelectric multiferroic material is formed. In the magnetic material, the arrangement direction of magnetic moments can be switched by an external magnetic field, and in the ferroelectric material, the electric field can regulate and control the ferroelectric polarization. The development of magnetoelectric multiferroic materials and the magnetoelectric coupling effect enable magnetic field regulation and electric polarization to obtain electric field regulation and magnetic moment direction. The mutual regulation and control between electromagnetism enables the same material to integrate multiple functions, provides possibility for miniaturization of devices, and has extremely high application prospect. Meanwhile, the appearance of multiferroic materials provides possibility for data multi-state storage. As is well known, our current data storage is mainly magnetic storage, and the storage state of the data storage is only + M state and-M state, so that the current computers and the like are 2-system storage. The development of the multi-iron material can effectively promote the rapid development of data storage, and the quaternary storage device can be developed based on four polarization states (+ M, + P), (+ M, -P), (-M, + P), (-M, -P) of the multi-iron material; the data storage density is greatly improved. In addition, the electromagnetic mutual control realized in the multiferroic material can realize ferroelectric writing and magnetic reading modes, and effectively solves the defects of slow writing and high energy consumption of the current magnetic storage.
However, similar to the current difficulties of superconductors, the application of multiferroic materials is limited because the magnetic/ferroelectric ordering temperature of multiferroic materials is extremely low, usually below-200 ℃.
Unlike the prior reports of medium-low temperature multiferroic materials, the Ba prepared by the invention4SmFe0.5Nb9.5O30Exhibits room temperature multiferroic property, shows ferromagnetic/ferroelectric coexistence at room temperature, and provides possibility for application of magnetoelectric multiferroic materials.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a room-temperature multiferroic material Ba4SmFe0.5Nb9.5O30The preparation method of (1). Ba obtained by the preparation method of the invention4SmFe0.5Nb9.5O30The material is crystallized into tungsten bronze, the sample particles are flaky, the large surface area of the sample particles provides convenience for interface defects, and Ba is beneficial to4SmFe0.5Nb9.5O30At room temperatureAnd generating ferromagnetism.
In order to solve the technical problems, the invention adopts the following technical scheme:
room-temperature multiferroic material Ba4SmFe0.5Nb9.5O30The preparation method comprises the following steps: (1) weighing: weighing appropriate amount of BaCO3、Sm2O3、Fe2O3And Nb2O5；
(2) Grinding: grinding the mixture with the metering ratio in the step (1) in an agate mortar for 6-10 hours;
(3) and (3) calcining: placing the uniformly mixed material obtained by grinding into Al2O3Placing the crucible made of the material in a muffle furnace, heating to 1100 ℃, and preserving heat for 5 hours;
(4) and (3) cooling: cooling the calcined sample at a slow rate to room temperature;
(5) and (3) secondary grinding: the cooled sample is reground for 2 to 4 hours;
(6) and (3) sintering: heating the sample after the secondary grinding to 1320-1370 ℃, wherein the sintering time is 4-6 hours;
(7) cooling the sintered sample to room temperature to obtain Ba4SmFe0.5Nb9.5O30Novel room temperature multiferroic materials.
Further, BaCO in the step (1)3,、Sm2O3、Fe2O3And Nb2O5The ratio of the amounts of the substances (A) to (B) is 16:2:1: 19.
Further, the temperature increase rate in the step (3) is 5 ℃/min.
Further, the cooling rate in the step (4) is 1-3 ℃/min.
Further, the temperature increase rate in the step (6) is 3 ℃/min.
Further, the sintering temperature in the step (6) is 1350 ℃, and the sintering time is 5 hours.
Further, the temperature reduction rate in the step (7) is 1 ℃/min.
By using saidRoom temperature multiferroic material Ba prepared by preparation method4SmFe0.5Nb9.5O30。
The room temperature multiferroic material Ba4SmFe0.5Nb9.5O30The crystal of (a) is a tungsten bronze structure, is a flaky particle and shows multiferroic characteristics at room temperature.
The invention has the beneficial effects that: the invention discloses a novel room-temperature multiferroic material Ba4SmFe0.5Nb9.5O30The crystal is of a tungsten bronze structure, the sample is flaky particles, and the coexistence characteristics of ferromagnetism and ferroelectricity are shown at room temperature. In addition, the preparation process is simple, the cost is low, and mass production can be realized.
Drawings
FIG. 1 shows a Ba of a room temperature multiferroic material of example 1 of the present invention4SmFe0.5Nb9.5O30XRD spectrum and SEM picture of (a).
FIG. 2 shows a Ba of a room temperature multiferroic material in example 1 of the present invention4SmFe0.5Nb9.5O30A hysteresis loop at room temperature M-H.
FIG. 3 shows a Ba of a room temperature multiferroic material in example 1 of the present invention4SmFe0.5Nb9.5O30The room temperature hysteresis loop P-E diagram.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
The novel room temperature multiferroic material Ba of the embodiment4SmFe0.5Nb9.5O30The preparation method comprises the following steps:
(1) BaCO with the ratio of the weighed material amounts of 16:2:1:193、Sm2O3、Fe2O3And Nb2O5；
(2) Grinding the mixture with the metering ratio in the step (1) in an agate mortar for 6 hours;
(3) placing the uniformly mixed material obtained by grinding into Al2O3Placing the crucible in a muffle furnace, heating to 1100 ℃ at the heating rate of 5 ℃/min, and preserving heat for 5 hours;
(4) cooling the calcined sample to room temperature at a slow rate of 1 ℃/minute;
(5) regrinding the sample for 3 hours;
(6) heating the sample subjected to secondary grinding to 1350 ℃ at the speed of 3 ℃/min, and preserving heat for 5 hours;
(7) cooling the sample to room temperature at the speed of 1 ℃/min after heat preservation to obtain Ba4SmFe0.5Nb9.5O30Novel room temperature multiferroic materials.
For Ba prepared in the above example4SmFe0.5Nb9.5O30And (3) representing the microstructure and the morphology of the material sample, analyzing the phase of the material sample by adopting an X-ray diffractometer (XRD), and representing the morphology of the material sample by adopting a field emission Scanning Electron Microscope (SEM). As can be seen from the main graph of FIG. 1, the sample has sharp diffraction peak, good crystallization and no other impurities; as can be seen from the inset in fig. 1, the samples crystallized as plate-like particles with a higher surface area to volume ratio.
FIG. 2 shows a new room temperature multiferroic material Ba4SmFe0.5Nb9.5O30A hysteresis loop at room temperature M-H. It can be seen from the figure that there is a clear loop in the M-H curve at room temperature for the sample, confirming its room temperature ferromagnetic properties.
FIG. 3 shows a Ba, a novel room temperature multiferroic material, in example 1 of the present invention4SmFe0.5Nb9.5O30The room temperature hysteresis loop P-E diagram. The non-linear P-E curve demonstrates its room temperature ferroelectric properties.
Example 2
The novel room temperature multiferroic material Ba of the embodiment4SmFe0.5Nb9.5O30The preparation method comprises the following steps:
(1) weighing the amount of the substanceBaCO at a ratio of 16:2:1:193, Sm2O3, Fe2O3, Nb2O5；
(2) Grinding the mixture with the metering ratio in the step (1) in an agate mortar for 10 hours;
(3) placing the uniformly mixed material obtained by grinding into Al2O3Placing the crucible in a muffle furnace, heating to 1100 ℃ at the heating rate of 5 ℃/min, and preserving heat for 10 hours;
(4) cooling the calcined sample to room temperature at a slow rate of 2 ℃/min;
(5) regrinding the sample for 2 hours;
(6) heating the sample after the secondary grinding to 1320 ℃ at the speed of 3 ℃/min, and preserving the heat for 6 hours;
(7) naturally cooling the sample to room temperature at the speed of 1 ℃/minute after heat preservation to obtain Ba4SmFe0.5Nb9.5O30Novel room temperature multiferroic materials.
Example 3
The novel room temperature multiferroic material Ba of the embodiment4SmFe0.5Nb9.5O30The preparation method comprises the following steps:
(1) weighing BaCO at a metering ratio of 16:2:1:193, Sm2O3, Fe2O3, Nb2O5；
(2) Putting the mixture with the metering ratio in the step (1) into an agate mortar for grinding for 8 hours;
(3) placing the uniformly mixed material obtained by grinding into Al2O3Placing the crucible in a muffle furnace, heating to 1100 ℃ at the heating rate of 5 ℃/min, and preserving heat for 5 hours;
(4) cooling the calcined sample to room temperature at a slow rate of 3 ℃/min;
(5) regrinding the sample for 4 hours;
(6) heating the sample subjected to secondary grinding to 1350 ℃ at the speed of 3 ℃/min, and preserving heat for 5 hours;
(7) will preserve heat and then sampleThe product was cooled to room temperature at a rate of 1 deg.C/min to obtain Ba4SmFe0.5Nb9.5O30Novel room temperature multiferroic materials.
Example 4
The novel room temperature multiferroic material Ba of the embodiment4SmFe0.5Nb9.5O30The preparation method comprises the following steps:
(1) weighing BaCO at a metering ratio of 16:2:1:193, Sm2O3, Fe2O3, Nb2O5；
(2) Grinding the mixture with the metering ratio in the step (1) in an agate mortar for 9 hours;
(3) placing the uniformly mixed material obtained by grinding into Al2O3Placing the crucible in a muffle furnace, heating to 1100 ℃ at the heating rate of 5 ℃/min, and preserving heat for 5 hours;
(4) cooling the calcined sample to room temperature at a slow rate of 3 ℃/min;
(5) regrinding the sample for 2 hours;
(6) heating the sample subjected to secondary grinding to 1370 ℃ at the speed of 3 ℃/min, and preserving heat for 4 hours;
(7) cooling the sample to room temperature at the speed of 1 ℃/min after heat preservation to obtain Ba4SmFe0.5Nb9.5O30Novel room temperature multiferroic materials.
The foregoing shows and describes the general principles and features of the present invention, together with the advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (9)
1. Room-temperature multiferroic material Ba4SmFe0.5Nb9.5O30The preparation method is characterized by comprising the following steps: weighing: weighing appropriate amount of BaCO3、Sm2O3、 Fe2O3And Nb2O5；
(2) Grinding: grinding the mixture with the metering ratio in the step (1) in an agate mortar for 6-10 hours;
(3) and (3) calcining: placing the uniformly mixed material obtained by grinding into Al2O3Placing the crucible made of the material in a muffle furnace, heating to 1100 ℃, and preserving heat for 5 hours;
(4) and (3) cooling: cooling the calcined sample at a slow rate to room temperature;
(5) and (3) secondary grinding: the cooled sample is reground for 2 to 4 hours;
(6) and (3) sintering: heating the sample after the secondary grinding to 1320-1370 ℃, wherein the sintering time is 4-6 hours;
(7) cooling the sintered sample to room temperature to obtain Ba4SmFe0.5Nb9.5O30Novel room temperature multiferroic materials.
2. The type room temperature multiferroic material Ba of claim 14SmFe0.5Nb9.5O30The preparation method is characterized by comprising the following steps: BaCO in the step (1)3,、Sm2O3、Fe2O3And Nb2O5The ratio of the amounts of the substances (A) to (B) is 16:2:1: 19.
3. The room temperature multiferroic material Ba of claim 14SmFe0.5Nb9.5O30The preparation method is characterized by comprising the following steps: the heating rate in the step (3) is 5 ℃/min.
4. The room temperature multiferroic material Ba of claim 14SmFe0.5Nb9.5O30The preparation method is characterized by comprising the following steps: the cooling rate in the step (4) is 1-3 ℃/min.
5. The room temperature multiferroic material Ba of claim 14SmFe0.5Nb9.5O30The preparation method is characterized by comprising the following steps: the temperature rise rate in the step (6) is 3 ℃/min.
6. The room temperature multiferroic material Ba of claim 14SmFe0.5Nb9.5O30The preparation method is characterized by comprising the following steps: the sintering temperature in the step (6) is 1350 ℃, and the sintering time is 5 hours.
7. The room temperature multiferroic material Ba of claim 14SmFe0.5Nb9.5O30The preparation method is characterized by comprising the following steps: the cooling rate in the step (7) is 1 ℃/min.
8. Room temperature multiferroic material Ba prepared by the preparation method of any one of claims 1-74SmFe0.5Nb9.5O30。
9. The room temperature multiferroic material Ba of claim 84SmFe0.5Nb9.5O30The method is characterized in that: the room temperature multiferroic material Ba4SmFe0.5Nb9.5O30The crystal of (a) is a tungsten bronze structure, is a flaky particle and shows multiferroic characteristics at room temperature.
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| CN114874009A (en) * | 2022-06-09 | 2022-08-09 | 郑州轻工业大学 | Near-room temperature relaxation ferroelectric material Ba 4 SrBiTi 3 Nb 7 O 30 And preparation method and application thereof |
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| JP2010255121A (en) * | 2010-07-20 | 2010-11-11 | Mitsubishi Heavy Ind Ltd | Film material |
| CN106478096A (en) * | 2015-08-31 | 2017-03-08 | 中国民航大学 | A kind of rare earth base novel non-full of type tungsten bronze ferroelectric material and preparation method thereof |
| CN107986784A (en) * | 2017-12-04 | 2018-05-04 | 福州大学 | A kind of tungsten bronze pure phase room temperature multiferroic ceramic thick film and preparation method thereof |
| CN108675789A (en) * | 2018-06-27 | 2018-10-19 | 桂林理工大学 | A kind of new iron-based ceramic capacitor material and preparation method thereof |
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| JP2010255121A (en) * | 2010-07-20 | 2010-11-11 | Mitsubishi Heavy Ind Ltd | Film material |
| CN106478096A (en) * | 2015-08-31 | 2017-03-08 | 中国民航大学 | A kind of rare earth base novel non-full of type tungsten bronze ferroelectric material and preparation method thereof |
| CN107986784A (en) * | 2017-12-04 | 2018-05-04 | 福州大学 | A kind of tungsten bronze pure phase room temperature multiferroic ceramic thick film and preparation method thereof |
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| CN114874009A (en) * | 2022-06-09 | 2022-08-09 | 郑州轻工业大学 | Near-room temperature relaxation ferroelectric material Ba 4 SrBiTi 3 Nb 7 O 30 And preparation method and application thereof |
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