CN114988861A - Hexagonal rare earth iron oxide single-phase multiferroic material and preparation method and application thereof - Google Patents
Hexagonal rare earth iron oxide single-phase multiferroic material and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of hexagonal rare earth iron oxide single-phase multiferroic materials, and discloses a hexagonal rare earth iron oxide single-phase multiferroic material and a preparation method and application thereof; the material is hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 As a matrix, and passing In 3+ Hexagonal rare earth doped iron oxide Lu 0.5 Sc 0.5 FeO 3 Zhonglu (Chinese Lu) 3+ Is obtained and has the molecular formula (Lu) 1‑x In x ) 0.5 Sc 0.5 FeO 3 Wherein x is In 3+ And x is more than or equal to 10 mol% and less than or equal to 40 mol%. The preparation method is simple and convenient, has low preparation cost and low requirement on instruments and equipment, is suitable for industrial production, and the obtained (Lu) is prepared by the method 1‑x In x ) 0.5 Sc 0.5 FeO 3 The material has excellent performance, can be used as a single-phase multiferroic functional material, and can even be used as a functional material for magnetoelectric coupling, high-density storage and the like after being explored.
Description
Technical Field
The invention relates to the technical field of hexagonal rare earth iron oxide single-phase multiferroic materials, in particular to a hexagonal rare earth iron oxide single-phase multiferroic material and a preparation method and application thereof.
Background
In the modern society, with the continuous development of information society, the demand of people for high-density data storage media is pressing, and especially, a storage media with high-efficiency, low-cost and sufficient data storage capacity plays a crucial role in the development of current information technology. Multiferroic materials are important functional materials that have two or more basic iron sequences among ferromagnetism, ferroelectricity, ferroelasticity, and ferrovorticity. There are coupling effects between the basic iron sequences in these materials, such as: the material realizes the electric field control magnetism or the magnetic field control electric polarization, realizes the regulation and control among various degrees of freedom and is applied, thereby greatly improving the storage density of the storage medium and having wide application prospect in the fields of high-density storage and the like.
Hexagonal rare earth iron oxide (h-RFeO) 3 ) Is a novel single-phase multiferroic material, which is a geometric ferroelectric, and the ferroelectricity comes from geometric resistance measures, namely FeO in the material 5 The bipyramid undergoes a relative displacement that the structural distortion-induced R-site ions cannot counteract. The system structure distortion necessarily causes the change of magnetic exchange between iron ions, and shows the strong magnetic coupling effect. Therefore, the hexagonal rare earth iron oxide is a very promising multiferroic material, has great application prospect in the fields of magnetoelectric sensor devices, high-density memory devices and the like,
although the hexagonal rare-earth iron oxide system has a high ferroelectric phase transition temperature, the magnetic phase transition of the system is too low, and the magnetization intensity is low. At present, few reports are made on the hexagonal rare earth iron oxide system, and therefore, it is very important to provide a novel compound of the hexagonal rare earth iron oxide system. Although the prior art proposes that the preparation of hexagonal iron oxide can be realized through epitaxial stress, the preparation process has high requirements and is not beneficial to popularization and application.
Therefore, the invention provides a hexagonal rare earth iron oxide single-phase multiferroic material, and a preparation method and application thereof.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a hexagonal rare earth iron oxide single-phase multiferroic material, and a preparation method and application thereof.
The hexagonal rare earth iron oxide single-phase multiferroic material and the preparation method and the application thereof are realized by the following technical scheme:
the first purpose of the invention is to provide a hexagonal rare earth iron oxide single-phase multiferroic material, which is prepared from hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 As a matrix, and passing In 3+ Hexagonal rare earth doped iron oxide Lu 0.5 Sc 0.5 FeO 3 Zhonglu (Chinese Lu) 3+ Is obtained and has the molecular formula (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 ;
Wherein x is In 3+ And x is more than or equal to 10 mol% and less than or equal to 40 mol%.
Further, In 3+ The doping concentration x is more than or equal to 10 mol% and less than or equal to 20 mol%.
The second purpose of the invention is to provide a preparation method of the hexagonal rare earth iron oxide single-phase multiferroic material, which is characterized by comprising the following steps:
step 1, according to the molecular formula (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 Respectively weighing a Lu source, an In source, a Sc source, a Fe source and an O source according to the stoichiometric ratio In the formula (I), and uniformly mixing to obtain mixed powder;
and 3, grinding the precursor material, pressing into tablets, and sintering at 1300-1500 ℃ for 12-36 h to obtain the hexagonal rare earth iron oxide single-phase multiferroic material.
Further, the Lu source, the In source, the Sc source and the Fe source are all oxides containing corresponding elements, and the O source is provided by oxygen In each oxide containing corresponding elements.
Further, in the step 2, the time of the pre-sintering treatment is 8-16 h, and the heating rate is 3-10 ℃/min.
Further, in the step 2, the time of the secondary pre-sintering treatment is 8-16 h, and the temperature rise rate is 3-10 ℃/min.
Further, in the step 3, the compression pressure of the pressed tablet is 15-25 Mpa, and the pressure maintaining time is 5-10 min.
Further, in the step 3, the temperature rise rate of the sintering treatment is 3-10 ℃/min.
The third purpose of the invention is to provide the application of the hexagonal rare earth iron oxide single-phase multiferroic material in the preparation of magnetic-electric sensing devices and high-density storage devices.
Compared with the prior art, the invention has the following beneficial effects:
the hexagonal rare earth iron oxide single-phase multiferroic material (Lu) of the invention 1-x In x ) 0.5 Sc 0.5 FeO 3 The performance is excellent, the magnetic transformation is shown near 163K, the spin reorientation is shown at low temperature, another magnetic phase transformation exists at a high-temperature section, and meanwhile, the magnetic phase transformation temperature is increased to room temperature along with the increase of the doping amount, so that the magnetic phase transformation temperature of the system is greatly increased; the hexagonal rare earth iron oxide single-phase multiferroic material of the invention shows hysteresis phenomenon at room temperature, also shows that the material shows magnetic ordering phenomenon at room temperature, and shows that the In-doped hexagonal rare earth iron oxide single-phase multiferroic material can be used as a single-phase multiferroic functional material, and even can be used as a functional material for magnetoelectric coupling, high-density storage and the like after being explored。
The invention adopts the hexagonal LuFeO 3 The system is specifically composed of hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 As a matrix, by selecting In 3+ The radius of doped ion is larger than that of In 3+ Lu of 3+ (under the same coordination conditions) thereby enhancing K in the system 3 The shape structure is distorted, so that Lu can be increased 0.5 Sc 0.5 FeO 3 The magnetic phase transition temperature of the system; and with In 3+ Increase in doping amount, System K 3 The structural distortion will be increased, and the magnetic phase transition temperature of the system will not be reduced.
The preparation method is simple and convenient, has low preparation cost and low requirement on instruments and equipment, and is suitable for industrial production.
Drawings
Fig. 1 is an XRD pattern of hexagonal rare earth iron oxide single-phase multiferroic material of example 1 and example 2 of the present invention, wherein x-0.1 is the XRD pattern of example 1 and x-0.2 is the XRD pattern of example 2;
fig. 2 is XRD patterns of hexagonal rare earth iron oxide single-phase multiferroic materials of examples 3 and 4 of the present invention, wherein x-0.3 is the XRD pattern of example 3 and x-0.4 is the XRD pattern of example 4;
fig. 3 is SEM images of hexagonal rare earth iron oxide single-phase multiferroic materials of example 1 and example 2 of the present invention, wherein x is 0.1 is SEM image of example 1, and x is 0.2 is SEM image of example 2;
fig. 4 is SEM images of hexagonal rare earth iron oxide single-phase multiferroic materials of example 3 and example 4, wherein x 0.3 is SEM image of example 3, and x 0.4 is SEM image of example 4;
fig. 5 is a graph showing the variation of magnetization with temperature of the hexagonal rare earth iron oxide single-phase multiferroic material according to the present invention, wherein fig. 5(a) is a graph showing the variation of magnetization with temperature of example 1, fig. 5(b) is a graph showing the variation of magnetization with temperature of example 2, fig. 5(c) is a graph showing the variation of magnetization with temperature of example 3, and fig. 5(d) is a graph showing the variation of magnetization with temperature of example 4;
FIG. 6 is a graph showing the variation of magnetization intensity with external field of hexagonal rare earth iron oxide single-phase multiferroic material of the present invention, FIG. 6(a) is a graph showing the variation of magnetization intensity with external field at 300K, and FIG. 6(b) is a graph showing the variation of magnetization intensity with external field at 200K; where x is 0.1, x is 0.2, x is 0.3, and x is 0.4, the magnetization of example 1 changes with the external field.
Detailed Description
As described in the background art, the preparation process of the hexaferrite oxide in the prior art is very strict, which results in a great difficulty in preparing the novel hexaferrite oxide, and is not favorable for the research on the performance thereof by the skilled person. For bulk rare earth iron oxide, the stable structure is an orthogonal structure, and it is difficult to prepare a stable hexagonal polar structure, but the inventors found that a hexagonal structure, such as Lu of the hexagonal structure, can be induced by suitable small radius ion doping to provide suitable chemical pressure 1-x Sc x FeO 3 (0.4<x<0.7). Therefore, the invention provides a hexagonal rare earth iron oxide single-phase multiferroic material, and a preparation method and application thereof.
The technical scheme in the embodiment of the invention is clearly and completely described in the following with reference to the attached drawings in the embodiment of the invention. In the present invention 3+ The doping concentration of (A) means In 3+ Relative to Lu 0.5 Sc 0.5 FeO 3 Zhonglu (Chinese Lu) 3+ The percentage of locations.
Example 1
This example provides a hexagonal rare earth iron oxide single-phase multiferroic material, which is prepared from hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 As a matrix, and passing In 3+ Hexagonal rare earth doped iron oxide Lu 0.5 Sc 0.5 FeO 3 Lu of Chinese medicine 3+ Obtained in situ and having the molecular formula (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 Wherein x is In 3+ X is 10 mol%. And the book is trueThe preparation method of the hexagonal rare-earth iron oxide single-phase multiferroic material of the embodiment is as follows:
step 1, according to the molecular formula (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 Respectively weighing Lu according to the stoichiometric ratio in 2 O 3 , In 2 O 3 ,Sc 2 O 3 ,Fe 2 O 3 Oxide powder, and grinding and uniformly mixing the oxide powder to obtain mixed powder;
in this example, Lu 2 O 3 ,In 2 O 3 ,Sc 2 O 3 ,Fe 2 O 3 The purity of the oxide powder is more than 99.99%.
In this example, the specific form of grinding is not limited as long as each raw material can be mixed uniformly. In this embodiment, a mechanical grinding method may be optionally used for grinding, for example, mechanical ball milling is performed until the particle size of the mixed powder is 1 to 5 μm.
in this embodiment, specific temperature increase rates of the pre-sintering treatment and the secondary sintering treatment are not limited, and the temperature increase may be stabilized. In this embodiment, the heating rates of the optional pre-sintering treatment and the secondary sintering treatment are both 5 ℃/min.
In this embodiment, the product after the pre-sintering treatment is ground and then subjected to the secondary pre-sintering treatment, and the specific mode of the grinding treatment after the pre-sintering treatment is not limited in this embodiment as long as the obtained product can be ground into uniform powder. In the embodiment, a mechanical grinding mode can be optionally adopted for grinding until the grain size of the pre-sintering treatment product is 1-5 microns, so that the pre-sintering treatment product can be prevented from being uniformly heated in the secondary pre-sintering treatment process, and the condition that the final performance of the material is not completely influenced by incomplete sintering is avoided.
In this embodiment, the pre-sintered product may be optionally cooled to room temperature at a cooling rate of 5 ℃/min and then ground.
Step 3, maintaining the pressure for 8min under the pressure of 20Mpa after the precursor material is ground, pressing into tablets, and sintering at the temperature of 1400 ℃ for 24h to obtain the hexagonal rare earth iron oxide single-phase multiferroic material;
it should be noted that the specific manner of the precursor material grinding process is not limited in this embodiment, as long as the obtained product can be ground into a uniform powder. In the embodiment, a mechanical grinding mode is optionally adopted for grinding until the particle size of the precursor material is 1-5 μm, so that the precursor material can be uniformly heated in a sintering treatment process after being pressed into tablets, and the hexagonal rare earth iron oxide single-phase multiferroic material with uniform components is obtained.
In this embodiment, the precursor material may be optionally cooled to room temperature at a cooling rate of 5 ℃/min and then ground. And in the step 3, the temperature rise rate of the sintering treatment is 5 ℃/min.
Example 2
This example provides a hexagonal rare earth iron oxide single-phase multiferroic material, which is prepared from hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 As a matrix, and passing In 3+ Hexagonal rare earth doped iron oxide Lu 0.5 Sc 0.5 FeO 3 Lu of Chinese medicine 3+ Position derived and having the formula (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 Wherein x is In 3+ X is 20 mol%. The preparation method of the hexagonal rare earth iron oxide single-phase multiferroic material of the embodiment is as follows:
step 1, according to the molecular formula (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 Respectively weighing Lu according to the stoichiometric ratio in 2 O 3 , In 2 O 3 ,Sc 2 O 3 ,Fe 2 O 3 Oxide powder, and grinding and uniformly mixing the oxide powder to obtain mixed powder;
in this embodiment, Lu 2 O 3 ,In 2 O 3 ,Sc 2 O 3 ,Fe 2 O 3 The purity of the oxide powder is more than 99.99%.
In this example, the specific form of grinding is not limited as long as each raw material can be mixed uniformly. In this embodiment, ball milling may be optionally used to grind the powder mixture until the particle size of the powder mixture is 1 to 5 μm.
in this embodiment, specific temperature increase rates of the pre-sintering treatment and the secondary sintering treatment are not limited, and the temperature increase may be stabilized. In this embodiment, the heating rates of the optional pre-sintering treatment and the secondary sintering treatment are both 5 ℃/min.
In this embodiment, the product after the pre-sintering treatment is ground and then subjected to the secondary pre-sintering treatment, and the specific mode of the grinding treatment after the pre-sintering treatment is not limited in this embodiment as long as the obtained product can be ground into uniform powder. In the embodiment, ball milling can be optionally adopted until the particle size of the presintering treatment product is 1-5 μm.
In this embodiment, the pre-sintered product may be optionally cooled to room temperature at a cooling rate of 5 ℃/min and then ground.
Step 3, maintaining the pressure for 8min under the pressure of 20Mpa after the precursor material is ground, pressing into tablets, and sintering at the temperature of 1400 ℃ for 24h to obtain the hexagonal rare earth iron oxide single-phase multiferroic material;
it should be noted that the specific manner of the precursor material grinding process is not limited in this embodiment, as long as the obtained product can be ground into a uniform powder. In the embodiment, ball milling can be optionally adopted until the particle size of the precursor material is 1-5 μm.
In this embodiment, the precursor material may be optionally cooled to room temperature at a cooling rate of 5 ℃/min, and then ground. And in the step 3, the temperature rise rate of the sintering treatment is 5 ℃/min.
Example 3
This example provides a hexagonal rare earth iron oxide single-phase multiferroic material, which is prepared from hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 As a matrix, and passing In 3+ Hexagonal rare earth doped iron oxide Lu 0.5 Sc 0.5 FeO 3 Lu of Chinese medicine 3+ Position derived and having the formula (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 Wherein x is In 3+ X is 30 mol%. The preparation method of the hexagonal rare earth iron oxide single-phase multiferroic material of the embodiment is as follows:
step 1, according to the molecular formula (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 The Lu is weighed respectively according to the stoichiometric ratio 2 O 3 , In 2 O 3 ,Sc 2 O 3 ,Fe 2 O 3 Oxide powder, and grinding and uniformly mixing the oxide powder to obtain mixed powder;
in this example, Lu 2 O 3 ,In 2 O 3 ,Sc 2 O 3 ,Fe 2 O 3 The purity of the oxide powder is more than 99.99%.
In this example, the specific form of grinding is not limited as long as each raw material can be mixed uniformly. In this embodiment, ball milling may be optionally used to grind the powder mixture until the particle size of the powder mixture is 1 to 5 μm.
in this embodiment, the specific temperature increase rates of the pre-sintering treatment and the secondary sintering treatment are not limited as long as the temperature increase is stable. In this embodiment, the heating rates of the optional pre-sintering treatment and the secondary sintering treatment are both 5 ℃/min.
In this embodiment, the product after the pre-sintering treatment is ground and then subjected to the secondary pre-sintering treatment, and the specific mode of the grinding treatment after the pre-sintering treatment is not limited in this embodiment as long as the obtained product can be ground into uniform powder. In the embodiment, ball milling can be optionally adopted until the particle size of the presintering treatment product is 1-5 μm.
In this embodiment, the heating rates of the optional pre-sintering treatment and the secondary sintering treatment are both 5 ℃/min, and the product after the pre-sintering treatment is cooled to room temperature by adopting the cooling rate of 5 ℃/min, and then is ground.
Step 3, maintaining the pressure for 8min under the pressure of 20Mpa after the precursor material is ground, pressing into tablets, and sintering at the temperature of 1400 ℃ for 24h to obtain the hexagonal rare earth iron oxide single-phase multiferroic material;
it should be noted that the specific manner of the precursor material grinding process is not limited in this embodiment, as long as the obtained product can be ground into a uniform powder. In the embodiment, ball milling can be optionally adopted until the particle size of the precursor material is 1-5 μm.
In this embodiment, the precursor material may be optionally cooled to room temperature at a cooling rate of 5 ℃/min, and then ground. And in the step 3, the temperature rise rate of the sintering treatment is 5 ℃/min.
Example 4
This example provides a hexagonal rare earth iron oxide single-phase multiferroic material, which is hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 As a matrix, and passing In 3+ Hexagonal rare earth doped iron oxide Lu 0.5 Sc 0.5 FeO 3 Lu of Chinese medicine 3+ Position derived and having the formula (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 Wherein x is In 3+ X is 40 mol%. The preparation method of the hexagonal rare earth iron oxide single-phase multiferroic material of the embodiment is as follows:
step 1, according to the molecular formula (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 The Lu is weighed respectively according to the stoichiometric ratio 2 O 3 , In 2 O 3 ,Sc 2 O 3 ,Fe 2 O 3 Oxide powder, and grinding and mixing the oxide powder uniformly to obtain mixed powder;
in this embodiment, Lu 2 O 3 ,In 2 O 3 ,Sc 2 O 3 ,Fe 2 O 3 The purity of the oxide powder is more than 99.99%.
In this example, the specific form of grinding is not limited as long as each raw material can be mixed uniformly. In this embodiment, ball milling may be optionally adopted for grinding until the particle size of the mixed powder is 1-5 μm.
in this embodiment, the specific temperature increase rates of the pre-sintering treatment and the secondary sintering treatment are not limited as long as the temperature increase is stable. In this embodiment, the heating rates of the optional pre-sintering treatment and the secondary sintering treatment are both 5 ℃/min.
In this embodiment, the product after the pre-sintering treatment is ground and then subjected to the secondary pre-sintering treatment, and the specific mode of the grinding treatment after the pre-sintering treatment is not limited in this embodiment as long as the obtained product can be ground into uniform powder. In the embodiment, ball milling can be optionally adopted until the particle size of the pre-sintered product is 1-5 μm.
In this embodiment, the pre-sintered product may be optionally cooled to room temperature at a cooling rate of 5 ℃/min and then ground.
Step 3, after grinding the precursor material, maintaining the pressure for 8min under the pressure of 20Mpa, pressing the precursor material into a tablet, and then sintering the tablet at the temperature of 1400 ℃ for 24h to obtain the hexagonal rare earth iron oxide single-phase multiferroic material;
it should be noted that the specific manner of the precursor material grinding process is not limited in this embodiment, as long as the obtained product can be ground into a uniform powder. In the embodiment, ball milling can be optionally adopted until the particle size of the precursor material is 1-5 μm.
In this embodiment, the precursor material may be optionally cooled to room temperature at a cooling rate of 5 ℃/min and then ground. And in the step 3, the temperature rise rate of the sintering treatment is 5 ℃/min.
Example 5
The present example differs from example 1 only in that:
in step 2 in this embodiment, the temperature rise rate of the pre-sintering treatment and the temperature rise rate of the secondary sintering treatment are both 3 ℃/min, and the product after the pre-sintering treatment is cooled to room temperature by using the temperature reduction rate of 3 ℃/min, and then is ground.
In step 3 of this embodiment, the precursor material is cooled to room temperature at a cooling rate of 3 ℃/min, and then ground. And in the step 3, the temperature rise rate of the sintering treatment is 3 ℃/min.
Example 6
The present example differs from example 1 only in that:
in step 2 in this embodiment, the temperature rise rate of the pre-sintering treatment and the temperature rise rate of the secondary sintering treatment are both 10 ℃/min, and the product after the pre-sintering treatment is cooled to room temperature by using the temperature reduction rate of 10 ℃/min, and then is ground.
In step 3 of this embodiment, the precursor material is cooled to room temperature at a cooling rate of 10 ℃/min, and then ground. And in step 3, the heating rate of the sintering treatment is 10 ℃/min.
Test section
The present inventors obtained sample 1, sample 2, sample 3 and sample 4 by taking 2g of the precursor materials obtained in examples 1 to 4, respectively, and pressing them into tablets by the methods of examples 1 to 4, respectively, according to the methods of examples 1 to 4, and recorded that x is 0.1, x is 0.2, x is 0.3 and x is 0.4, respectively.
(I) XRD test
In the present invention, sample 1, sample 2, sample 3 and sample 4 are subjected to room temperature XRD tests, and the results are shown as x being 0.1 and x being 0.2 in fig. 1, and x being 0.3 and x being 0.4 in fig. 2, respectively.
As can be seen from fig. 1 and 2: the XRD diffraction peaks of the sample 1, the sample 2, the sample 3 and the sample 4 are quite consistent with the XRD data of the hexagonal rare earth iron oxide, and are all in a polar hexagonal structure, and the space group is P6 3 cm, indicating that all samples are ferroelectric at room temperature.
(II) SEM test
The present invention performs SEM test on sample 1, sample 2, sample 3 and sample 4, and the test results are shown in fig. 3 where x is 0.1 and x is 0.2, and fig. 4 where x is 0.3 and x is 0.4, respectively.
As can be seen from fig. 3 and 4: the microstructures of sample 1, sample 2, sample 3 and sample 4 all showed uniform grain size and good compactness, with average grain size of about 5 μm. Only sample 4 had abnormally grown grains.
(III) magnetic Property measurement
In the present invention, sample 1, sample 2, sample 3 and sample 4 were subjected to magnetic property tests, and the test results are shown in fig. 5 and fig. 6, where x is 0.1, 0.2, 0.3 and 0.4, respectively.
Fig. 5 is a graph showing the change of magnetization with temperature of the hexagonal rare earth iron oxide single-phase multiferroic material of the present invention, wherein fig. 5(a) is a graph showing the change of magnetization with temperature of sample 1, fig. 5(b) is a graph showing the change of magnetization with temperature of sample 2, fig. 5(c) is a graph showing the change of magnetization with temperature of sample 3, and fig. 5(d) is a graph showing the change of magnetization with temperature of sample.
As can be seen from fig. 5: all samples showed complex magnetic phase transition, and it is known from the reported hexagonal rare earth iron oxide multiferroic material that magnetic transition is shown near 163K, and spin reorientation is also shown at low temperature. In addition, all samples have another magnetic phase transition in a high-temperature section, and the magnetic phase transition temperature is increased to room temperature along with the increase of the doping amount, so that the magnetic phase transition temperature of the system is greatly increased.
Fig. 6 is a graph showing the variation of magnetization with external field of the hexagonal rare earth iron oxide single-phase multiferroic material according to the present invention, and fig. 6(a) and 6(b) are graphs showing the variation of magnetization with external field at 300K and 200K, respectively.
As can be seen from the figure: when the In doping amount In the sample is increased to 0.4, the hexagonal rare earth iron oxide multiferroic material shows a hysteresis phenomenon at room temperature, and the material also shows a magnetic ordering phenomenon at room temperature. Therefore, the In-doped hexagonal rare earth iron oxide single-phase multiferroic material shows more excellent room-temperature magnetic performance, and the development of the hexagonal rare earth iron oxide single-phase multiferroic material is greatly promoted.
It is to be understood that the above-described embodiments are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Claims (9)
1. The hexagonal rare earth iron oxide single-phase multiferroic material is characterized in that hexagonal rare earth iron oxide Lu is used 0.5 Sc 0.5 FeO 3 As a matrix, and passing In 3+ Hexagonal rare earth doped iron oxide Lu 0.5 Sc 0.5 FeO 3 Zhonglu (Chinese Lu) 3+ Is obtained in the position of (A) and has the molecular formula of (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 ;
Wherein x is In 3+ And x is more than or equal to 10 mol% and less than or equal to 40 mol%.
2. The hexagonal rare earth iron oxide single-phase multiferroic material of claim 1, In 3+ The doping concentration x is more than or equal to 10 mol% and less than or equal to 20 mol%.
3. A method for preparing a hexagonal rare earth iron oxide single-phase multiferroic material according to claim 1 or 2, comprising the steps of:
step 1, according to the molecular formula (Lu) 1-x In x ) 0.5 Sc 0.5 FeO 3 Respectively weighing a Lu source, an In source, a Sc source, an Fe source and an O source according to the stoichiometric ratio, and uniformly mixing to obtain mixed powder;
step 2, performing pre-sintering treatment on the obtained mixed powder at the temperature of 900-1100 ℃, and then performing secondary pre-sintering treatment at the temperature of 1150-1350 ℃ to obtain a precursor material;
and 3, grinding the precursor material, pressing into tablets, and sintering at 1300-1500 ℃ for 12-36 h to obtain the hexagonal rare earth iron oxide single-phase multiferroic material.
4. The production method according to claim 3, wherein the Lu source, the In source, the Sc source, and the Fe source are each an oxide containing a corresponding element, and the O source is provided by oxygen In each of the oxides containing a corresponding element.
5. The preparation method according to claim 3, wherein in the step 2, the time of the pre-sintering treatment is 8-16 h, and the temperature rise rate is 3-10 ℃/min.
6. The preparation method according to claim 3, wherein in the step 2, the time of the secondary pre-sintering treatment is 8-16 h, and the temperature rise rate is 3-10 ℃/min.
7. The method according to claim 3, wherein in step 3, the tablet is compressed under a pressure of 15 to 25MPa for a pressure-holding time of 5 to 10 min.
8. The method according to claim 3, wherein in the step 3, the temperature increase rate of the sintering treatment is 3 to 10 ℃/min.
9. Use of the hexagonal rare-earth iron oxide single-phase multiferroic material according to claim 1 or 2 in the preparation of a magneto-electric sensor device and a high-density memory device.
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