CN112877811A - Preparation method of perovskite type rare earth oxide magnetic nano material - Google Patents

Preparation method of perovskite type rare earth oxide magnetic nano material Download PDF

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CN112877811A
CN112877811A CN202110207951.6A CN202110207951A CN112877811A CN 112877811 A CN112877811 A CN 112877811A CN 202110207951 A CN202110207951 A CN 202110207951A CN 112877811 A CN112877811 A CN 112877811A
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rare earth
raw material
10mmol
perovskite type
earth oxide
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胡全丽
岳斌
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Inner Mongolia University for Nationlities
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F9/00Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
    • D01F9/08Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/0036Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties showing low dimensional magnetism, i.e. spin rearrangements due to a restriction of dimensions, e.g. showing giant magnetoresistivity
    • H01F1/0045Zero dimensional, e.g. nanoparticles, soft nanoparticles for medical/biological use
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties

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Abstract

The invention discloses a preparation method of a perovskite type rare earth oxide magnetic nano material, which prepares a perovskite type rare earth oxide by using an electrostatic spinning technology, wherein the crystal structure of the perovskite type rare earth oxide is an orthorhombic system, the material appearance is nanofiber, and the perovskite type rare earth oxide magnetic nano material has better magnetic performance at different temperatures. By adopting the method provided by the invention to prepare the magnetic material, the magnetic material shows uniformity and has good surface appearance, and can be widely applied to the technical field of functional materials.

Description

Preparation method of perovskite type rare earth oxide magnetic nano material
Technical Field
The invention relates to the field of functional materials, in particular to a preparation method of a perovskite type rare earth oxide magnetic nano material.
Background
The magnetic material is used as the basis of national economy and national defense industry and is widely applied to information storage industries such as telecommunication, communication and the like. The magnetism is mainly divided into paramagnetic, superparamagnetic, ferromagnetic, antiferromagnetic, diamagnetic, and the like. The magnetic nano material has unique magnetic properties, such as superparamagnetism, high coercivity, high magnetic susceptibility and the like. The superparamagnetic material can be applied to the field of aerospace and has important application in magnetic resonance imaging and disease diagnosis. The ferromagnetic material can be used as a permanent magnetic material and a magnetic recording material and applied to the technical field of power electronics. Perovskite type rare earth-transition metal oxide RMO3Has the characteristics of stable structure, rich oxygen vacancy and the like. RMO3The magnetic material is derived from transition metal ions M3+And rare earth ion R3+The magnetic phenomenon of the material is richer due to the multiple spin arrangement modes of electrons. Common RMO3The magnetic material synthesis method mainly comprises a solid-phase sintering method and a sol-gel method, and the product has poor crystallinity, irregular appearance and more surface defects.
Therefore, a device capable of overcoming the above-mentioned drawbacks is yet to be proposed.
Disclosure of Invention
Aiming at the problems, the invention provides a method for preparing a perovskite type rare earth oxide nano material with magnetic property by utilizing an electrostatic spinning technology. The product prepared by the process has the advantages of high crystallinity, regular appearance, less surface defects, good crystal orientation, uniform nanofiber appearance, good magnetic property and the like. The process method provided by the invention is simple and flexible, and has low cost.
In order to achieve the purpose, the technical scheme provided by the invention is as follows:
a preparation method of a perovskite type rare earth oxide magnetic nano material comprises the steps of preparing a perovskite type rare earth oxide by an electrostatic spinning technology, wherein the crystal structure of the perovskite type rare earth oxide is an orthorhombic system, the material appearance is nanofiber, and the perovskite type rare earth oxide magnetic nano material has good magnetic properties at different temperatures, and specifically comprises the following steps:
1) weighing a proper amount of polyvinylpyrrolidone, and accurately weighing a compound raw material containing rare earth R and a compound raw material containing transition metal M according to the element molar ratio R: M being 1: 1.
2) Placing the compound raw material containing rare earth and the compound raw material containing transition metal weighed in the step 1) into a beaker, placing the polyvinylpyrrolidone weighed in the step 1) into the beaker, adding a proper amount of N, N-dimethylformamide, and stirring for 4-20 hours at room temperature by using a magnetic stirrer to form a uniform solution;
3) transferring the solution formed in the step 2) into a glass injector, and preparing a magnetic material precursor by an electrostatic spinning process under the conditions of room temperature, voltage of 13-18kV, injection speed of 0.4-1.0ml/h and receiving distance of 15-30 cm;
4) putting the precursor prepared in the step 3) into a muffle furnace, calcining for 2-4 hours at the air condition of 500-800 ℃, and cooling to obtain a target product.
Preferably, the polyvinylpyrrolidone weighed in the step 1) is 5g, the N, N-dimethylformamide is 45ml, the weighed compound raw material containing the rare earth R is 10mmol of samarium nitrate, and the compound raw material containing the transition metal M is 10mmol of iron acetate.
Preferably, the polyvinylpyrrolidone weighed in the step 1) is 5g, the N, N-dimethylformamide is 45ml, the weighed compound raw material containing the rare earth R is 10mmol of samarium nitrate, and the compound raw material containing the transition metal M is 10mmol of cobalt acetate.
Preferably, the polyvinylpyrrolidone weighed in the step 1) is 5g, the N, N-dimethylformamide is 45ml, the raw material of the compound containing the rare earth R is 10mmol of neodymium nitrate, and the raw material of the compound containing the transition metal M is 10mmol of ferric acetate.
Preferably, the polyvinylpyrrolidone weighed in the step 1) is 5g, the N, N-dimethylformamide is 45ml, the raw material of the compound containing the rare earth R is 10mmol of neodymium nitrate, and the raw material of the compound containing the transition metal M is 10mmol of cobalt acetate.
Preferably, the polyvinylpyrrolidone weighed in the step 1) is 5g, the N, N-dimethylformamide is 45ml, the raw material of the compound containing the rare earth R is 10mmol of neodymium nitrate, and the raw material of the compound containing the transition metal M is 10mmol of nickel acetate.
Compared with the prior art, the invention has the advantages that:
the product prepared by the method provided by the invention has uniform nanofiber appearance and good magnetic property; the method is simple and flexible, has low cost, and can economically and efficiently produce the magnetic nanofiber material.
Drawings
FIG. 1 is SmFeO prepared in example one3X-ray diffraction patterns of (a);
FIG. 2 is SmCoO prepared in example II3X-ray diffraction patterns of (a);
FIG. 3 shows NdFeO prepared in example III3X-ray diffraction patterns of (a);
FIG. 4 shows NdCoO prepared in example IV3X-ray diffraction patterns of (a);
FIG. 5 shows NdNiO prepared in example V3X-ray diffraction patterns of (a);
FIG. 6 shows SmFeO prepared in example one3Scanning electron microscope images of;
FIG. 7 is SmCoO prepared in example two3Scanning electron microscope images of;
FIG. 8 shows NdFeO produced in EXAMPLE III3Scanning electron microscope images of;
FIG. 9 shows NdCoO prepared in example IV3Scanning electron microscope images of;
FIG. 10 shows NdNiO prepared in example V3Scanning electron microscope images of;
FIG. 11 is SmFeO prepared in example one3The hysteresis loop of (1);
FIG. 12 is SmCoO prepared in example two3The hysteresis loop of (1);
FIG. 13 shows NdFeO produced in EXAMPLE III3The hysteresis loop of (1);
FIG. 14 shows NdCoO prepared in EXAMPLE four3The hysteresis loop of (1);
FIG. 15 shows NdNiO prepared in example V3The hysteresis loop of (1).
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The invention provides a preparation method of a perovskite type rare earth oxide magnetic nano material, which has good magnetic property and uniform nanofiber appearance, and specifically comprises the following steps:
1) weighing a proper amount of polyvinylpyrrolidone, and accurately weighing a compound raw material containing rare earth R and a compound raw material containing transition metal M respectively according to the element molar ratio R: M being 1: 1;
2) placing the compound raw material containing rare earth and the compound raw material containing transition metal weighed in the step 1) into a beaker, placing the polyvinylpyrrolidone weighed in the step 1) into the beaker, adding a proper amount of N, N-dimethylformamide, and stirring for 4-20 hours at room temperature by using a magnetic stirrer to form a uniform solution;
3) transferring the solution formed in the step 2) into a glass injector, and preparing a magnetic material precursor by an electrostatic spinning process under the conditions of room temperature, voltage of 13-18kV, injection speed of 0.4-1.0ml/h and receiving distance of 15-30 cm;
4) putting the precursor prepared in the step 3) into a muffle furnace, calcining for 2-4 hours at the air condition of 500-800 ℃, and cooling to obtain a target product.
The method provided by the present invention is further illustrated below with reference to specific examples.
Example one
Weighing 10mmol of samarium nitrate as a compound raw material containing rare earth R, placing the samarium nitrate in a beaker, weighing 10mmol of iron acetate as a compound raw material containing transition metal M, adding the iron acetate in the beaker, weighing 5g of polyvinylpyrrolidone in the beaker, weighing 45ml of N, N-dimethylformamide in the beaker, and stirring for 4-20 hours at room temperature by using a magnetic stirrer to form a uniform dark brown solution;
transferring the solution into an injector, and preparing a precursor material by an electrostatic spinning process under the conditions of the room temperature, the voltage of 13-18kV, the injection speed of 0.4-1.0ml/h and the receiving distance of 15-30 cm;
the prepared precursor material is put into a muffle furnace, calcined for 2 to 4 hours under the air condition of 500-800 ℃, and cooled to obtain the nano fibrous perovskite SmFeO3A magnetic material. FIG. 1 is SmFeO prepared3The analysis shows that the prepared material is consistent with standard card PDF #39-1490, belongs to an orthorhombic system, and has a space group Pnma (62). In SmFeO3The morphology of the sample can be seen as a uniform nanofiber structure in the scanning electron microscope image (fig. 6). FIG. 11 shows SmFeO3Hysteresis loops at different temperatures, material tablesExhibits ferromagnetism.
Example two
Weighing 10mmol of samarium nitrate as a compound raw material containing rare earth R in a beaker, weighing 10mmol of cobalt acetate as a compound raw material containing transition metal M in the beaker, weighing 10mmol of cobalt acetate in the beaker, weighing 5g of polyvinylpyrrolidone in the beaker, and weighing 45ml of N, N-dimethylformamide in the beaker;
stirring for 4-20 hours at room temperature by using a magnetic stirrer to form a uniform dark purple solution; transferring the solution into an injector, and preparing a precursor material by an electrostatic spinning process under the conditions of the room temperature, the voltage of 13-18kV, the injection speed of 0.4-1.0ml/h and the receiving distance of 15-30 cm;
the prepared precursor material is put into a muffle furnace, calcined for 2 to 4 hours under the air condition of 500-800 ℃, and cooled to obtain the nano fibrous perovskite SmCoO3A magnetic material. FIG. 2 is SmCoO prepared3The analysis shows that the prepared material is consistent with standard card PDF #25-1071, belongs to an orthorhombic system and has a space group of Pbnm (62). SmCoO3The morphology of the sample can be seen as a uniform nanofiber structure in the scanning electron microscope image (fig. 7). FIG. 12 is SmCoO3The material shows superparamagnetism at 298K and 50K temperature and weak ferromagnetism at 5K temperature in a hysteresis loop at different temperatures.
EXAMPLE III
Weighing 10mmol of neodymium nitrate and putting the neodymium nitrate in a beaker, weighing 10mmol of ferric acetate and the compound containing transition metal M, adding the 10mmol of ferric acetate in the beaker, weighing 5g of polyvinylpyrrolidone in the beaker, weighing 45ml of N, N-dimethylformamide in the beaker, and stirring for 4-20 hours at room temperature by using a magnetic stirrer to form a uniform dark brown solution;
transferring the solution into an injector, and preparing a precursor material by an electrostatic spinning process under the conditions of the room temperature, the voltage of 13-18kV, the injection speed of 0.4-1.0ml/h and the receiving distance of 15-30 cm;
the prepared precursor material is put into a muffle furnaceCalcining for 2-4 hours at the temperature of 500-3A magnetic material. FIG. 3 is an X-ray diffraction pattern of the prepared NdFeO3, and analysis shows that the prepared material is in accordance with standard card PDF #25-1149, belongs to the orthorhombic system, and has a space group Pnma (62). NdFeO3The scanning electron microscope image of (2) can see that the morphology of the sample is a uniform nanofiber structure (fig. 8). FIG. 13 shows NdFeO3Hysteresis loops at different temperatures, the material exhibits paramagnetism at low temperatures and weak ferromagnetism at room temperature.
Example four
A compound raw material containing rare earth R is neodymium nitrate, and 10mmol of neodymium nitrate is weighed and placed in a beaker; a compound raw material containing transition metal M is cobalt acetate, and 10mmol of cobalt acetate is weighed and added into a beaker; weighing 5g of polyvinylpyrrolidone and adding the polyvinylpyrrolidone into a beaker; weighing 45ml of N, N-dimethylformamide, adding the N, N-dimethylformamide into a beaker, and stirring the N, N-dimethylformamide for 4 to 20 hours at room temperature by using a magnetic stirrer to form a uniform dark purple solution;
transferring the solution into an injector, and preparing a precursor material by an electrostatic spinning process under the conditions of the room temperature, the voltage of 13-18kV, the injection speed of 0.4-1.0ml/h and the receiving distance of 15-30 cm; the prepared precursor material is put into a muffle furnace, calcined for 2 to 4 hours under the air condition of 500-800 ℃, and cooled to obtain the nano fibrous perovskite NdCoO3A magnetic material. FIG. 4 shows NdCoO thus prepared3The analysis shows that the prepared material is consistent with standard card PDF #89-0551, belongs to an orthorhombic system and has a space group Pnma (62). NdCoO3The morphology of the sample can be seen as a uniform nanofiber structure in the scanning electron microscope image (fig. 9). FIG. 14 shows NdCoO3The material exhibits paramagnetism in the hysteresis loop at different temperatures.
EXAMPLE five
A compound raw material containing rare earth R is neodymium nitrate, and 10mmol of neodymium nitrate is weighed and placed in a beaker; a compound raw material containing transition metal M is nickel acetate, and 10mmol of nickel acetate is weighed and added into a beaker; weighing 5g of polyvinylpyrrolidone and adding the polyvinylpyrrolidone into a beaker; weighing 45ml of N, N-dimethylformamide and adding the N, N-dimethylformamide into a beaker; stirring for 4-20 hours at room temperature by using a magnetic stirrer to form a uniform green solution;
transferring the solution into an injector, and preparing a precursor material by an electrostatic spinning process under the conditions of the room temperature, the voltage of 13-18kV, the injection speed of 0.4-1.0ml/h and the receiving distance of 15-30 cm;
the prepared precursor material is put into a muffle furnace, calcined for 2 to 4 hours under the air condition of 500-800 ℃, and cooled to obtain the nano fibrous perovskite NdNiO3A magnetic material. FIG. 5 shows the NdNiO thus prepared3The analysis shows that the prepared material is consistent with standard card PDF #79-2457, belongs to an orthorhombic system and has a space group of Pbnm (62). NdNiO3The morphology of the sample can be seen as a uniform nanofiber structure in the scanning electron microscope image (fig. 10). FIG. 15 shows NdCoO3The material exhibits paramagnetism in the hysteresis loop at different temperatures.
The present invention and its embodiments have been described above, without limitation, and the embodiments shown in the drawings are only one of the embodiments of the present invention, and the actual organization is not limited thereto. In summary, those skilled in the art should appreciate that they can readily use the disclosed conception and specific embodiments as a basis for designing or modifying other structures for carrying out the same purposes of the present invention without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (6)

1. A preparation method of a perovskite type rare earth oxide magnetic nano material is characterized in that the crystal structure of the perovskite type rare earth oxide is an orthorhombic system, the material appearance is nanofiber, and the magnetic performance is shown at different temperatures, and the preparation method specifically comprises the following steps:
step 1) weighing a certain amount of polyvinylpyrrolidone, and accurately weighing a compound raw material containing rare earth R and a compound raw material containing transition metal M respectively according to the element molar ratio R: M being 1: 1;
step 2) placing the compound raw material containing rare earth and the compound raw material containing transition metal weighed in the step 1) into a beaker, placing the polyvinylpyrrolidone weighed in the step 1) into the beaker, adding a proper amount of N, N-dimethylformamide, and stirring for 4-20 hours at room temperature by using a magnetic stirrer to form a uniform solution;
step 3) transferring the solution formed in the step 2) into a glass injector, and preparing a magnetic material precursor by an electrostatic spinning process under the conditions of voltage of 13-18kV, injection speed of 0.4-1.0ml/h and receiving distance of 15-30cm at room temperature;
and 4) putting the precursor prepared in the step 3) into a muffle furnace, calcining for 2-4 hours at the temperature of 500-800 ℃, and cooling to obtain a target product.
2. The method for preparing a perovskite type rare earth oxide magnetic nanomaterial according to claim 1, wherein the polyvinylpyrrolidone weighed in the step 1) is 5g, the N, N-dimethylformamide is 45ml, the raw material of the compound containing rare earth R is 10mmol of samarium nitrate, and the raw material of the compound containing transition metal M is 10mmol of iron acetate.
3. The method for preparing a perovskite type rare earth oxide magnetic nanomaterial according to claim 1, wherein the polyvinylpyrrolidone weighed in the step 1) is 5g, the N, N-dimethylformamide is 45ml, the raw material of the compound containing rare earth R is 10mmol of samarium nitrate, and the raw material of the compound containing transition metal M is 10mmol of cobalt acetate.
4. The method for preparing a perovskite type rare earth oxide magnetic nanomaterial according to claim 1, wherein the polyvinylpyrrolidone weighed in the step 1) is 5g, the N, N-dimethylformamide is 45ml, the raw material of the compound containing rare earth R is 10mmol of neodymium nitrate, and the raw material of the compound containing transition metal M is 10mmol of ferric acetate.
5. The method for preparing a perovskite type rare earth oxide magnetic nanomaterial according to claim 1, wherein the polyvinylpyrrolidone weighed in the step 1) is 5g, the N, N-dimethylformamide is 45ml, the raw material of the compound containing rare earth R is 10mmol of neodymium nitrate, and the raw material of the compound containing transition metal M is 10mmol of cobalt acetate.
6. The method for preparing a perovskite type rare earth oxide magnetic nanomaterial according to claim 1, wherein the polyvinylpyrrolidone weighed in the step 1) is 5g, the N, N-dimethylformamide is 45ml, the raw material of the compound containing rare earth R is 10mmol of neodymium nitrate, and the raw material of the compound containing transition metal M is 10mmol of nickel acetate.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115128135A (en) * 2022-06-24 2022-09-30 泰山学院 Pb-doped SmFeO with hollow tubular structure 3 Gas-sensitive material and application thereof

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CN101235558A (en) * 2008-03-12 2008-08-06 长春理工大学 Method for preparing perovskite-type rare earth composite oxide porous hollow nano fiber
CN104313729A (en) * 2014-11-05 2015-01-28 大连交通大学 Double perovskite type inorganic nano fiber and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN101235558A (en) * 2008-03-12 2008-08-06 长春理工大学 Method for preparing perovskite-type rare earth composite oxide porous hollow nano fiber
CN104313729A (en) * 2014-11-05 2015-01-28 大连交通大学 Double perovskite type inorganic nano fiber and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN115128135A (en) * 2022-06-24 2022-09-30 泰山学院 Pb-doped SmFeO with hollow tubular structure 3 Gas-sensitive material and application thereof

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Application publication date: 20210601