CN116655365B - Hexagonal rare earth iron oxide high-entropy single-phase multiferroic material, preparation and application thereof - Google Patents
Hexagonal rare earth iron oxide high-entropy single-phase multiferroic material, preparation and application thereof Download PDFInfo
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- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 title claims abstract description 291
- 239000000463 material Substances 0.000 title claims abstract description 107
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 90
- -1 rare earth iron oxide Chemical class 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000011159 matrix material Substances 0.000 claims abstract description 56
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000000126 substance Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims description 83
- 238000005245 sintering Methods 0.000 claims description 78
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 57
- 238000010438 heat treatment Methods 0.000 claims description 54
- 239000002243 precursor Substances 0.000 claims description 51
- 238000011282 treatment Methods 0.000 claims description 44
- 239000011812 mixed powder Substances 0.000 claims description 42
- 229910052760 oxygen Inorganic materials 0.000 claims description 19
- 238000000227 grinding Methods 0.000 claims description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 13
- 239000001301 oxygen Substances 0.000 claims description 13
- 238000005303 weighing Methods 0.000 claims description 12
- 238000003825 pressing Methods 0.000 claims description 8
- 230000000630 rising effect Effects 0.000 claims 2
- 239000003826 tablet Substances 0.000 claims 2
- 239000007891 compressed tablet Substances 0.000 claims 1
- 230000006835 compression Effects 0.000 claims 1
- 238000007906 compression Methods 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 5
- 230000005621 ferroelectricity Effects 0.000 abstract description 3
- 230000005389 magnetism Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 235000013980 iron oxide Nutrition 0.000 description 80
- 238000000498 ball milling Methods 0.000 description 15
- 239000002245 particle Substances 0.000 description 14
- 230000005291 magnetic effect Effects 0.000 description 11
- 239000002994 raw material Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001816 cooling Methods 0.000 description 8
- 239000000047 product Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000005415 magnetization Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000008878 coupling Effects 0.000 description 4
- 238000010168 coupling process Methods 0.000 description 4
- 238000005859 coupling reaction Methods 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000007670 refining Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000005302 magnetic ordering Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
- C04B35/2675—Other ferrites containing rare earth metals, e.g. rare earth ferrite garnets
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Abstract
The invention belongs to the technical field of hexagonal rare earth iron oxide single-phase multiferroic materials and high entropy, and discloses a hexagonal rare earth iron oxide high entropy single-phase multiferroic material, and preparation and application thereof, wherein the hexagonal rare earth iron oxide Lu is used as the material 0.5 Sc 0.5 FeO 3 And Yb 0.5 In 0.5 FeO 3 Is a matrix obtained by mixing and doping it by introducing chemical pressure and has a molecular formula of (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 . The preparation method disclosed by the invention is simple to operate, low in preparation cost, easy to realize preparation conditions and requirements, and suitable for quantitative production and preparation; the hexagonal rare earth iron oxide single-phase multiferroic material prepared by the method has excellent performance, has ferroelectricity and magnetism near room temperature, and can be used as an excellent single-phase multiferroic functional material, a magneto-electric sensor, a high-density storage functional material and the like.
Description
Technical Field
The invention relates to the technical field of hexagonal rare earth iron oxide single-phase multiferroic materials and high entropy, in particular to a hexagonal rare earth iron oxide high entropy single-phase multiferroic material, and preparation and application thereof.
Background
The main focus of multiferroics research is coexistence and coupling between the ferroelectric sequence and the spin sequence, and the control of the electric polarization by using an external electric field to control the magnetic sequence or an external magnetic field is realized, so that the cross regulation and control between the magnetism and the electricity are achieved. The discovery of multiferroics and magnetoelectric coupling combines two major materials of ferroelectricity and magnetism which lack intrinsic relation traditionally, realizes the coupling of ferroelectric sequences and ferromagnetic sequences, integrates the physical advantages of two ordered phases in sequence, and provides a material basis for realizing applications such as polymorphic storage, electrographic magnetic reading and the like.
Hexagonal rare earth iron oxide systems, although having a high ferroelectric phase transition temperature, have too low a magnetic phase transition and a low magnetization. At present, few reports about a hexagonal rare earth iron oxide system are provided, and the preparation of the hexagonal iron oxide through epitaxial stress is proposed in the prior art, but the preparation process has high requirements, is not beneficial to manufacturing blocks and is not beneficial to popularization and use.
Therefore, the invention provides a hexagonal rare earth iron oxide high-entropy 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 high-entropy single-phase multiferroic material, and a preparation method and application thereof. The invention adopts a high entropy strategy, leads multi-component elements into the hexagonal rare earth iron oxide matrix, and finely adjusts the performance of the hexagonal rare earth iron oxide matrix by adjusting the concentration of the components to obtain the hexagonal rare earth iron oxide (Yb) 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 The hexagonal rare earth iron oxide obtained by the invention is a novel high-entropy single-phase multiferroic material, is a high-entropy material with high entropy characteristics, is a ferroelectric material with geometric measure, and has a plurality of basic iron orders.
The invention relates to a hexagonal rare earth iron oxide high-entropy single-phase multiferroic material and a preparation method and application thereof, which are realized by the following technical scheme:
the first object of the present invention is to provide a hexagonal rare earth iron oxide high entropy single phase multiferroic material prepared from hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 And Yb 0.5 In 0.5 FeO 3 Is a matrix obtained by mixing and doping it by introducing chemical pressure and has a molecular formula of (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 。
The second object of the invention is to provide a preparation method of the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material, which comprises the following steps:
step 1, lu is used 0.5 Sc 0.5 FeO 3 And Yb 0.5 In 0.5 FeO 3 Is used as a matrix, and is sintered at 1300-1450 ℃ after being uniformly mixed to obtain a precursor;
wherein the matrix Lu 0.5 Sc 0.5 FeO 3 And the matrix Yb 0.5 In 0.5 FeO 3 The molar ratio of (2) is 1:1;
and 2, grinding the precursor, pressing the precursor into a tablet, and sintering the precursor at 1350-1500 ℃ to obtain the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material.
Further, in the step 1, the sintering time of the sintering treatment is 12-18 hours, and the heating rate is 4-6 ℃/min.
In step 2, the sintering time of the sintering treatment is 12-18 h, and the heating rate is 4-6 ℃/min.
Further, in the step 2, the pressurizing pressure of the pressed tablet is 15-20 Mpa, and the pressure maintaining time is 8-12 min.
Further, in step 1, the Lu 0.5 Sc 0.5 FeO 3 The method comprises the following steps:
according to hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 The stoichiometric ratio in the raw materials is respectively weighed corresponding to the massThe Lu source, the Sc source, the Fe source A and the O source A are uniformly mixed to obtain mixed powder A; subsequently, the mixed powder A is subjected to pre-sintering treatment I and secondary sintering treatment I in sequence to obtain matrix Lu 0.5 Sc 0.5 FeO 3 ；
Wherein the Lu source, the Sc source and the Fe source A are all oxides containing corresponding elements, and the O source A is provided by oxygen in each oxide containing the corresponding elements.
Further, the temperature of the presintering treatment I is 1000-1200 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min;
the temperature of the secondary sintering treatment I is 1300-1400 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min.
Further, in step 1, the Yb 0.5 In 0.5 FeO 3 The method comprises the following steps:
according to hexagonal rare earth iron oxide Yb 0.5 In 0.5 FeO 3 Respectively weighing Yb source, in source, fe source B and O source B with corresponding mass according to the stoichiometric ratio of the powder, and uniformly mixing the Yb source, the In source, the Fe source B and the O source B to obtain mixed powder B; then, the mixed powder B is subjected to pre-sintering treatment II and secondary sintering treatment II in sequence to obtain a matrix Yb 0.5 In 0.5 FeO 3 ；
Wherein, the Yb source, the In source and the Fe source B are all oxides containing corresponding elements, and the O source B is provided by oxygen In each oxide containing corresponding elements.
Further, the temperature of the presintering treatment II is 1100-1250 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min;
the temperature of the secondary sintering treatment II is 1300-1400 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min.
The third object of the invention is to provide an application of the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material in preparing magneto-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 high-entropy single-phase multiferroic material (Yb) 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 The hexagonal rare earth iron oxide single-phase high-entropy phase multiferroic material disclosed by the invention has excellent performance, not only shows magnetic transformation near 150K, but also shows spin reorientation at low temperature, and shows hysteresis at room temperature, and also shows that the material shows magnetic ordering at room temperature, so that the hexagonal rare earth iron oxide single-phase multiferroic material can be used as a single-phase multiferroic functional material, and is hopeful to be used as a functional material for magneto-electric coupling, high-density storage and the like.
The preparation method is simple and convenient, has low preparation cost, is low in equipment and equipment, and is suitable for industrial production.
Drawings
FIG. 1 is an XRD pattern of a hexagonal rare earth iron oxide high entropy single phase multiferroic material according to example 1 of the present invention;
FIG. 2 is an XRD pattern of the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material prepared by direct mixing in comparative example 1 of the present invention;
FIG. 3 is an SEM image of a hexagonal rare earth iron oxide high entropy single phase multiferroic material according to example 1 of the present invention;
FIG. 4 is a graph showing the magnetization of the hexagonal rare earth iron oxide high entropy single phase multiferroic material according to the present invention as a function of temperature;
FIG. 5 is a plot of magnetization of the hexagonal rare earth iron oxide high entropy single phase multiferroic material according to the present invention as a function of external field.
Detailed Description
As described in the background art, the preparation process of the hexagonal rare earth iron oxide in the prior art is very strict and less, so that the preparation of the novel hexagonal iron oxide is difficult and is not beneficial to the study of the performance of the novel hexagonal iron oxide by a person skilled in the art. For the bulk rare earth iron oxide, the stable structure is the same as the normal structure, and the stable hexagonal polar structure is difficult to prepare, but the inventor finds that a plurality of small-radius ions can be introduced into the composition through a high-entropy strategy to provide proper chemical pressure, and then the composition is carried outSuitable processing can induce hexagonal structures, such as hexagonal (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 . Therefore, the invention provides a hexagonal rare earth iron oxide high-entropy single-phase multiferroic material, and a preparation method and application thereof.
The invention provides a hexagonal rare earth iron oxide high-entropy single-phase multiferroic material, which is prepared by using hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 And Yb 0.5 In 0.5 FeO 3 Is a matrix obtained by mixing and doping it by introducing chemical pressure and has a molecular formula of (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 。
And the preparation method is as follows:
step 1, lu is used 0.5 Sc 0.5 FeO 3 And Yb 0.5 In 0.5 FeO 3 Is used as a matrix, and is sintered at 1300-1450 ℃ after being uniformly mixed to obtain a precursor;
step 2, grinding the precursor, pressing the precursor into a tablet, and sintering the precursor at 1350-1500 ℃ to obtain the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material;
in order to ensure that pure hexagonal rare earth iron oxide high-entropy single-phase multiferroic material can be obtained, the invention adopts a mode of multiple sintering treatments, preferably firstly uses a matrix Lu 0.5 Sc 0.5 FeO 3 With matrix Yb 0.5 In 0.5 FeO 3 Mixing in equimolar manner, and sintering to obtain Lu as matrix 0.5 Sc 0.5 FeO 3 With matrix Yb 0.5 In 0.5 FeO 3 After forming the precursor material, the precursor material is sintered again to ensure that a material having a molecular formula of (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 Is a hexagonal rare earth iron oxide high-entropy single-phase multiferroic material.
The sintering treatment process for preparing the precursor comprises the following steps: by combining the matrix Lu 0.5 Sc 0.5 FeO 3 With matrix Yb 0.5 In 0.5 FeO 3 After being evenly mixed, the mixture is heated to 1300-1450 ℃ at a heating rate of 4-6 ℃/min, and sintered for 12-18 h at the temperature of 1300-1450 ℃. In order to finally obtain a composition of uniform molecular formula (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 Is prepared from hexagonal rare-earth iron oxide, high-entropy single-phase multiferroic material, and Lu as matrix by grinding 0.5 Sc 0.5 FeO 3 With matrix Yb 0.5 In 0.5 FeO 3 Mixing uniformly to obtain matrix Lu 0.5 Sc 0.5 FeO 3 With matrix Yb 0.5 In 0.5 FeO 3 Mixing, and mixing.
The invention relates to a method for obtaining pure and homogeneous components of the formula (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 The hexagonal rare earth iron oxide high-entropy single-phase multiferroic material is characterized in that before the precursor is subjected to secondary sintering treatment, the precursor is ground until the particle size of the precursor is 1-5 mu m, so that after the precursor material is pressed into a tablet, the precursor material can be uniformly heated in the sintering treatment process, impurities or other byproducts are avoided, and the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material with uniform components is obtained. Wherein, the pressurizing pressure of the pressed tablet is 15-20 Mpa, and the pressure maintaining time is 8-12 min; the sintering treatment time is 12-18 h, and the heating rate is 4-6 ℃/min.
The invention can obtain the molecular formula (Yb) 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 The hexagonal rare earth iron oxide high-entropy single-phase multiferroic material is also required to be described, and the preferred Lu adopted in the invention 0.5 Sc 0.5 FeO 3 The method comprises the following steps:
according to hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 Respectively weighing Lu source, sc source, fe source A and O source A with corresponding mass, and uniformly mixing to obtain mixed powder A; then, the mixed powder A is subjected to pre-sintering treatment I and secondAfter the sintering treatment I, a matrix Lu is obtained 0.5 Sc 0.5 FeO 3 ；
The invention adopts the Lu source, the Sc source and the Fe source A as oxides containing corresponding elements, and the O source A is provided by oxygen in each oxide containing the corresponding elements.
The invention is not limited to the specific mixing mode of the Lu source, the Sc source, the Fe source A and the O source A, and all the preparation raw materials can be uniformly mixed, for example, the preparation raw materials can be optionally ground by adopting a mechanical grinding mode, such as mechanical ball milling until the particle size of the mixed powder A is 1-5 mu m, so that the pre-sintering treatment product can be uniformly heated in the second pre-sintering treatment process, and the condition that the final performance of the material is not thoroughly influenced by the sintering is avoided.
The Lu source, the Sc source, the Fe source A and the O source A are sintered in a sectional manner, namely, the pre-sintering treatment I and the secondary sintering treatment I are sequentially carried out, so that all elements can be fully and uniformly mixed in the sintering process, the condition of insufficient reaction among components is avoided, and a product with uniform components is obtained. Wherein the temperature of the presintering treatment I is 1000-1200 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min; the temperature of the secondary sintering treatment I is 1300-1400 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min.
And the Yb preferably used in the present invention 0.5 In 0.5 FeO 3 The method comprises the following steps:
according to hexagonal rare earth iron oxide Yb 0.5 In 0.5 FeO 3 Respectively weighing Yb source, in source, fe source B and O source B with corresponding mass according to the stoichiometric ratio of the powder, and uniformly mixing the Yb source, the In source, the Fe source B and the O source B to obtain mixed powder B; then, the mixed powder B is subjected to pre-sintering treatment II and secondary sintering treatment II in sequence to obtain a matrix Yb 0.5 In 0.5 FeO 3 ；
The Yb source, the In source and the Fe source B adopted by the invention are all oxides containing corresponding elements, and the O source B is provided by oxygen In each oxide containing the corresponding elements.
The invention is not limited to the specific mixing mode of the Yb source, the In source, the Fe source B and the O source B, and all the preparation raw materials can be uniformly mixed, for example, the preparation raw materials can be optionally ground by adopting a mechanical grinding mode, such as mechanical ball milling until the particle size of the mixed powder A is 1-5 mu m, so that the pre-sintering treatment II product can be heated uniformly In the secondary sintering treatment II process, and the condition that the final performance of the material is not thoroughly influenced by sintering is avoided.
The sectional sintering treatment is adopted for the Yb source, the In source, the Fe source B and the O source B, namely the sintering treatment is carried out In a mode of sequentially carrying out the pre-sintering treatment II and the secondary sintering treatment II, so that all elements can be fully and uniformly mixed In the sintering process, the condition of insufficient reaction among components is avoided, and the product with uniform components is obtained. Wherein the temperature of the presintering treatment II is 1100-1250 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min; the temperature of the secondary sintering treatment II is 1300-1400 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min.
Example 1
The embodiment provides a hexagonal rare earth iron oxide high-entropy single-phase multiferroic material, and the preparation method thereof is as follows:
step 1, preparing a matrix Lu 0.5 Sc 0.5 FeO 3 ：
1) According to hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 Respectively weighing Lu source, sc source, fe source A and O source A with corresponding mass, and uniformly mixing to obtain mixed powder A;
in this embodiment, the Lu source is Lu 2 O 3 The powder and Sc source are Sc 2 O 3 The powder and Fe source A are Fe 2 O 3 Powder, O source A is derived from Lu 2 O 3 Powder, sc 2 O 3 Powder and Fe 2 O 3 Oxygen in the powder, and Lu 2 O 3 Powder, sc 2 O 3 Powder and Fe 2 O 3 The purity of the powder is above 99.99%.
That is, the present embodimentIn (C) by mixing Lu 2 O 3 Powder, sc 2 O 3 Powder and Fe 2 O 3 And (3) carrying out mechanical ball milling on the powder, and carrying out mechanical ball milling until the particle size of the mixed powder A is 1-5 mu m, thus obtaining the mixed powder A.
2) Heating the obtained mixed powder A to 1200 ℃ at a heating rate of 5 ℃/min, presintering at 1200 ℃ for 12 hours, heating to 1350 ℃ at a heating rate of 5 ℃/min, sintering at 1350 ℃ for 12 hours, and cooling to room temperature to obtain matrix Lu 0.5 Sc 0.5 FeO 3 。
Step 2, preparing matrix Yb 0.5 In 0.5 FeO 3 ：
1) According to hexagonal rare earth iron oxide Yb 0.5 In 0.5 FeO 3 Respectively weighing Yb source, in source, fe source B and O source B according to the stoichiometric ratio of the raw materials, and uniformly mixing the Yb source, the In source, the Fe source B and the O source B to obtain mixed powder B;
in the present embodiment, the Yb source is Yb 2 O 3 The powder and In source is In 2 O 3 The powder and Fe source B are Fe 2 O 3 Powder, O source B is derived from Yb 2 O 3 Powder, in 2 O 3 Powder and Fe 2 O 3 Oxygen in powder, and Yb 2 O 3 Powder, in 2 O 3 Powder and Fe 2 O 3 The purity of the powder is above 99.99%.
That is, in the present embodiment, by incorporating Yb 2 O 3 Powder, in 2 O 3 Powder and Fe 2 O 3 And (3) carrying out mechanical ball milling on the powder, and carrying out mechanical ball milling until the particle size of the mixed powder A is 1-5 mu m, thus obtaining the mixed powder B.
2) Heating the obtained mixed powder B to 1200 ℃ at a heating rate of 5 ℃/min, presintering at 1200 ℃ for 12 hours, heating to 1350 ℃ at a heating rate of 5 ℃/min, sintering at 1350 ℃ for 12 hours, and cooling to room temperature to obtain the matrix Yb 0.5 In 0.5 FeO 3 。
Step 3, preparing a precursor:
the matrix Lu obtained in step 1 is subjected to 0.5 Sc 0.5 FeO 3 And the matrix Yb obtained in the step 2 0.5 In 0.5 FeO 3 Grinding, mixing uniformly, heating to 1400 ℃ at a heating rate of 5 ℃/min, and sintering at 1400 ℃ for 12 hours to obtain the precursor.
Step 4, preparing the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material
And (3) grinding the precursor material until the particle size of the precursor material is 1-5 mu m, pressing the precursor material into a tablet under the pressure of 20Mpa for 8min, heating the pressed tablet precursor to 1450 ℃ at the heating rate of 5 ℃/min, and sintering the precursor material at the temperature of 1450 ℃ for 12h to obtain the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material.
Example 2
The embodiment provides a hexagonal rare earth iron oxide high-entropy single-phase multiferroic material, and the preparation method thereof is as follows:
step 1, preparing a matrix Lu 0.5 Sc 0.5 FeO 3 ：
1) According to hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 Respectively weighing Lu source, sc source, fe source A and O source A with corresponding mass, and uniformly mixing to obtain mixed powder A;
in this embodiment, the Lu source is Lu 2 O 3 The powder and Sc source are Sc 2 O 3 The powder and Fe source A are Fe 2 O 3 Powder, O source A is derived from Lu 2 O 3 Powder, sc 2 O 3 Powder and Fe 2 O 3 Oxygen in the powder, and Lu 2 O 3 Powder, sc 2 O 3 Powder and Fe 2 O 3 The purity of the powder is above 99.99%.
That is, in the present embodiment, by adding Lu 2 O 3 Powder, sc 2 O 3 Powder and Fe 2 O 3 Mechanically ball milling the powder until the particle size of the mixed powder A is 1-5 mu m to obtainAnd obtaining mixed powder A.
2) Heating the obtained mixed powder A to 1000 ℃ at a heating rate of 4 ℃/min, presintering at 1000 ℃ for 18h, heating to 1300 ℃ at a heating rate of 4 ℃/min, sintering at 1300 ℃ for 18h, and cooling to room temperature to obtain matrix Lu 0.5 Sc 0.5 FeO 3 。
Step 2, preparing matrix Yb 0.5 In 0.5 FeO 3 ：
1) According to hexagonal rare earth iron oxide Yb 0.5 In 0.5 FeO 3 Respectively weighing Yb source, in source, fe source B and O source B according to the stoichiometric ratio of the raw materials, and uniformly mixing the Yb source, the In source, the Fe source B and the O source B to obtain mixed powder B;
in the present embodiment, the Yb source is Yb 2 O 3 The powder and In source is In 2 O 3 The powder and Fe source B are Fe 2 O 3 Powder, O source B is derived from Yb 2 O 3 Powder, in 2 O 3 Powder and Fe 2 O 3 Oxygen in powder, and Yb 2 O 3 Powder, in 2 O 3 Powder and Fe 2 O 3 The purity of the powder is above 99.99%.
That is, in the present embodiment, by incorporating Yb 2 O 3 Powder, in 2 O 3 Powder and Fe 2 O 3 And (3) carrying out mechanical ball milling on the powder, and carrying out mechanical ball milling until the particle size of the mixed powder A is 1-5 mu m, thus obtaining the mixed powder B.
2) Heating the obtained mixed powder B to 1100 ℃ at a heating rate of 4 ℃/min, presintering at 1100 ℃ for 18h, heating to 1300 ℃ at a heating rate of 4 ℃/min, sintering at 1300 ℃ for 18h, and cooling to room temperature to obtain the matrix Yb 0.5 In 0.5 FeO 3 。
Step 3, preparing a precursor:
the matrix Lu obtained in step 1 is subjected to 0.5 Sc 0.5 FeO 3 And the matrix Yb obtained in the step 2 0.5 In 0.5 FeO 3 The grinding is carried out and the grinding is carried out,mixing them uniformly, then raising the temperature to 1300 ℃ at a heating rate of 4 ℃/min, and sintering at 1300 ℃ for 18h to obtain the precursor.
Step 4, preparing the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material
And grinding the precursor material until the particle size of the precursor material is 1-5 mu m, pressing the precursor material into a tablet under the pressure of 15Mpa for 12min, heating the pressed tablet precursor to 1350 ℃ at the heating rate of 4 ℃/min, and sintering the precursor material at the temperature of 1350 ℃ for 18h to obtain the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material.
Example 3
The embodiment provides a hexagonal rare earth iron oxide high-entropy single-phase multiferroic material, and the preparation method thereof is as follows:
step 1, preparing a matrix Lu 0.5 Sc 0.5 FeO 3 ：
1) According to hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 Respectively weighing Lu source, sc source, fe source A and O source A with corresponding mass, and uniformly mixing to obtain mixed powder A;
in this embodiment, the Lu source is Lu 2 O 3 The powder and Sc source are Sc 2 O 3 The powder and Fe source A are Fe 2 O 3 Powder, O source A is derived from Lu 2 O 3 Powder, sc 2 O 3 Powder and Fe 2 O 3 Oxygen in the powder, and Lu 2 O 3 Powder, sc 2 O 3 Powder and Fe 2 O 3 The purity of the powder is above 99.99%.
That is, in the present embodiment, by adding Lu 2 O 3 Powder, sc 2 O 3 Powder and Fe 2 O 3 And (3) carrying out mechanical ball milling on the powder, and carrying out mechanical ball milling until the particle size of the mixed powder A is 1-5 mu m, thus obtaining the mixed powder A.
2) The mixed powder A obtained above is heated to 1100 ℃ at a heating rate of 6 ℃/min, and is presintered at 1100 ℃ for 16 hours, and then is subjected to a presintering treatment at a temperature of 6 ℃/miHeating the temperature of n to 1400 ℃, sintering at 1400 ℃ for 16h, and cooling to room temperature to obtain the matrix Lu 0.5 Sc 0.5 FeO 3 。
Step 2, preparing matrix Yb 0.5 In 0.5 FeO 3 ：
1) According to hexagonal rare earth iron oxide Yb 0.5 In 0.5 FeO 3 Respectively weighing Yb source, in source, fe source B and O source B according to the stoichiometric ratio of the raw materials, and uniformly mixing the Yb source, the In source, the Fe source B and the O source B to obtain mixed powder B;
in the present embodiment, the Yb source is Yb 2 O 3 The powder and In source is In 2 O 3 The powder and Fe source B are Fe 2 O 3 Powder, O source B is derived from Yb 2 O 3 Powder, in 2 O 3 Powder and Fe 2 O 3 Oxygen in powder, and Yb 2 O 3 Powder, in 2 O 3 Powder and Fe 2 O 3 The purity of the powder is above 99.99%.
That is, in the present embodiment, by incorporating Yb 2 O 3 Powder, in 2 O 3 Powder and Fe 2 O 3 And (3) carrying out mechanical ball milling on the powder, and carrying out mechanical ball milling until the particle size of the mixed powder A is 1-5 mu m, thus obtaining the mixed powder B.
2) Heating the obtained mixed powder B to 1250 ℃ at a heating rate of 6 ℃/min, presintering at 1250 ℃ for 16h, heating to 1400 ℃ at a heating rate of 6 ℃/min, sintering at 1400 ℃ for 16h, and cooling to room temperature to obtain the matrix Yb 0.5 In 0.5 FeO 3 。
Step 3, preparing a precursor:
the matrix Lu obtained in step 1 is subjected to 0.5 Sc 0.5 FeO 3 And the matrix Yb obtained in the step 2 0.5 In 0.5 FeO 3 Grinding, mixing uniformly, heating to 1450 ℃ at a heating rate of 6 ℃/min, and sintering at 1450 ℃ for 16h to obtain the precursor.
Step 4, preparing the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material
And grinding the precursor material until the particle size of the precursor material is 1-5 mu m, pressing the precursor material into a tablet under 18Mpa for 10min, heating the pressed tablet precursor to 1500 ℃ at a heating rate of 6 ℃/min, and sintering the precursor material at 1500 ℃ for 16h to obtain the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material.
Comparative example 1
The comparative example provides a hexagonal rare earth iron oxide material, and the preparation method thereof is as follows:
step 1, preparing a precursor:
1) According to hexagonal rare earth iron oxide (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 Respectively weighing a Lu source, a Yb source, a Sc source, a Fe source A and an O source with corresponding mass according to the stoichiometric ratio of the powder, and uniformly mixing and grinding the Lu source, the Yb source, the Sc source, the Fe source A and the O source to obtain mixed powder;
in this comparative example, the Yb source was Yb 2 O 3 The powder and Lu source is Lu 2 O 3 The powder and Sc source are Sc 2 O 3 The powder and Fe source is Fe 2 O 3 Powder, O source is from Lu 2 O 3 Powder, sc 2 O 3 Powder and Fe 2 O 3 Oxygen in the powder, and Lu 2 O 3 Powder, yb 2 O 3 、Sc 2 O 3 Powder and Fe 2 O 3 The purity of the powder is above 99.99%.
That is, in this comparative example, by incorporating Yb 2 O 3 Powder, lu 2 O 3 Powder, sc 2 O 3 Powder and Fe 2 O 3 And (3) carrying out mechanical ball milling on the powder, and carrying out mechanical ball milling until the particle size of the mixed powder is 1-5 mu m, thus obtaining the mixed powder.
2) Heating the obtained mixed powder to 1200 ℃ at a heating rate of 5 ℃/min, presintering at 1200 ℃ for 12h, cooling, fully grinding, heating to 1400 ℃ at a heating rate of 5 ℃/min, sintering at 1400 ℃ for 12h, coolingAfter cooling to room temperature, a precursor (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 。
Step 2, preparing hexagonal rare earth iron oxide material
And (3) grinding the precursor material until the particle size of the precursor material is 1-5 mu m, pressing the precursor material into a tablet under the pressure of 20Mpa for 8min, heating the pressed tablet precursor to 1450 ℃ at the heating rate of 5 ℃/min, and sintering at the temperature of 1450 ℃ for 12h to obtain the target product.
That is, this comparative example differs from example 1 in that: not using Lu 0.5 Sc 0.5 FeO 3 With Yb 0.5 In 0.5 FeO 3 Is prepared by mixing the substrates, but according to the target product (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 Directly sintering and doping the preparation raw materials.
Experimental part
XRD test
Taking the materials prepared in the example 1 and the comparative example 1 as examples, 2g of the materials are respectively pressed into tablets, and then XRD tests at room temperature are carried out on the materials, and the test results are shown in figures 1 and 2 respectively.
As can be seen from fig. 1: by comparing the references and refining with the hexagonal lattice constant in the literature, it was found that the XRD diffraction peaks of example 1 of the invention were very coincident with the XRD data of hexagonal rare earth iron oxide, and by refining the XRD data, polarity P6 appeared in the pattern 3 cm structure, the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material prepared in the embodiment 1 of the invention is of a polar hexagonal structure, and the space group is P6 3 cm, also shows that the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material prepared by the invention has ferroelectricity at room temperature.
As can be seen from fig. 2: by comparing the references and refining with the hexagonal lattice constants in the references, the Bragg diffraction peaks of obvious impurity phases appear near 27 degrees and 61 degrees of 2 theta, which shows that the material prepared in the comparative example 1 is not of a single-phase structure, obvious impurities exist, and pure hexagonal rare earth iron oxide high-entropy single-phase multiferroic material cannot be obtained.
As can be seen by comparing FIGS. 1 and 2, only the preparation method of the present invention, that is, the preparation of the matrix Lu, respectively, is performed first 0.5 Sc 0.5 FeO 3 With matrix Yb 0.5 In 0.5 FeO 3 And then the matrix Lu is added 0.5 Sc 0.5 FeO 3 With matrix Yb 0.5 In 0.5 FeO 3 Mixing, tabletting, and sintering to obtain pure and uniform molecular formula (Yb) 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 The theory part of the invention is verified, and the preparation method of the invention can avoid the generation of impurities or other byproducts, thereby effectively improving the performance of the prepared material.
(II) SEM test
The hexagonal rare earth iron oxide high-entropy single-phase multiferroic material prepared in example 1 is taken as an example for SEM test, and the test result is shown in FIG. 3.
As can be seen from fig. 3, the microstructure of the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material prepared in embodiment 1 of the present invention shows that the grain size is uniform, and the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material has good compactness, and further verifies that the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 。
(III) magnetic Performance test
FIG. 4 is a graph showing the magnetization of the hexagonal rare earth iron oxide high entropy single phase multiferroic material according to example 1 of the present invention as a function of temperature. And can be seen from fig. 4: the samples exhibit complex magnetic phase transitions, as known from the reported multiferroic materials of hexagonal rare earth iron oxides, magnetic transitions around 150K and spin reorientation at low temperatures. In addition, all samples also had another magnetic phase transition at the high temperature section.
Fig. 5 is a plot of magnetization of the hexagonal rare earth iron oxide high entropy single phase multiferroic material according to example 1 of the present invention as a function of external field. And can be seen from fig. 5: the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material of example 1 shows hysteresis at room temperature, and also shows that the material shows magnetic order at room temperature. Therefore, the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material can show more excellent room-temperature magnetic performance, and the development of the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material is greatly promoted.
In conclusion, the invention adopts a high entropy strategy, leads multi-component elements into the hexagonal rare earth iron oxide matrix, and finely adjusts the performance of the hexagonal rare earth iron oxide matrix by adjusting the concentration of the components to obtain the hexagonal rare earth iron oxide (Yb) 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 The hexagonal rare earth high-entropy iron oxide single-phase multiferroic material prepared by the invention can be used as a single-phase multiferroic functional material, is a high-entropy material with high entropy characteristics, and is a ferroelectric material with geometric measure, and a plurality of basic iron sequences exist in the material, so that the material prepared by the invention can be used as an excellent single-phase multiferroic functional material, a magneto-electric sensor, a high-density storage functional material and the like.
It should be apparent that the embodiments described above are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (10)
1. A hexagonal rare earth iron oxide high-entropy single-phase multiferroic material is characterized in that the hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 And Yb 0.5 In 0.5 FeO 3 Is a matrix obtained by mixing and doping it by introducing chemical pressure and has a molecular formula of (Yb 0.25 Lu 0.25 In 0.25 Sc 0.25 )FeO 3 ；
And it is prepared by the steps of:
step 1, lu is used 0.5 Sc 0.5 FeO 3 And Yb 0.5 In 0.5 FeO 3 Is used as a matrix, and is sintered at 1300-1450 ℃ after being uniformly mixed to obtain a precursor;
wherein the matrix Lu 0.5 Sc 0.5 FeO 3 And the matrix Yb 0.5 In 0.5 FeO 3 The molar ratio of (2) is 1:1;
and 2, grinding the precursor, pressing the precursor into a tablet, and sintering the precursor at 1350-1500 ℃ to obtain the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material.
2. A method for preparing the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material according to claim 1, which is characterized by comprising the following steps:
step 1, lu is used 0.5 Sc 0.5 FeO 3 And Yb 0.5 In 0.5 FeO 3 Is used as a matrix, and is sintered at 1300-1450 ℃ after being uniformly mixed to obtain a precursor;
wherein the matrix Lu 0.5 Sc 0.5 FeO 3 And the matrix Yb 0.5 In 0.5 FeO 3 The molar ratio of (2) is 1:1;
and 2, grinding the precursor, pressing the precursor into a tablet, and sintering the precursor at 1350-1500 ℃ to obtain the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material.
3. The method according to claim 2, wherein in step 1, the sintering time of the sintering treatment is 12 to 18 hours, and the temperature rising rate is 4 to 6 ℃/min.
4. The method according to claim 2, wherein in step 2, the sintering time of the sintering treatment is 12 to 18 hours, and the temperature rising rate is 4 to 6 ℃/min.
5. The method according to claim 2, wherein in step 2, the compression pressure of the compressed tablet is 15 to 20Mpa and the dwell time is 8 to 12min.
6. The method of claim 2, wherein in step 1, the Lu 0.5 Sc 0.5 FeO 3 The method comprises the following steps:
according to hexagonal rare earth iron oxide Lu 0.5 Sc 0.5 FeO 3 Respectively weighing Lu source, sc source, fe source A and O source A with corresponding mass, and uniformly mixing to obtain mixed powder A; subsequently, the mixed powder A is subjected to pre-sintering treatment I and secondary sintering treatment I in sequence to obtain matrix Lu 0.5 Sc 0.5 FeO 3 ；
Wherein the Lu source, the Sc source and the Fe source A are all oxides containing corresponding elements, and the O source A is provided by oxygen in each oxide containing the corresponding elements.
7. The preparation method according to claim 6, wherein the temperature of the presintering treatment I is 1000-1200 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min;
the temperature of the secondary sintering treatment I is 1300-1400 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min.
8. The method of claim 2, wherein in step 1, the Yb is selected from the group consisting of 0.5 In 0.5 FeO 3 The method comprises the following steps:
according to hexagonal rare earth iron oxide Yb 0.5 In 0.5 FeO 3 Respectively weighing Yb source, in source, fe source B and O source B with corresponding mass according to the stoichiometric ratio of the powder, and uniformly mixing the Yb source, the In source, the Fe source B and the O source B to obtain mixed powder B; then, the mixed powder B is subjected to pre-sintering treatment II and secondary sintering treatment II in sequence to obtain a matrix Yb 0.5 In 0.5 FeO 3 ；
Wherein, the Yb source, the In source and the Fe source B are all oxides containing corresponding elements, and the O source B is provided by oxygen In each oxide containing corresponding elements.
9. The preparation method according to claim 8, wherein the temperature of the presintering treatment II is 1100-1250 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min;
the temperature of the secondary sintering treatment II is 1300-1400 ℃, the sintering time is 12-18 h, and the heating rate is 4-6 ℃/min.
10. Use of the hexagonal rare earth iron oxide high-entropy single-phase multiferroic material according to claim 1 in the preparation of magneto-electric sensor devices and high-density memory devices.
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