CN112430078A - Preparation method of high-performance nano rare earth doped barium ferrite permanent magnet material - Google Patents
Preparation method of high-performance nano rare earth doped barium ferrite permanent magnet material Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-performance nano rare earth doped barium ferrite permanent magnetic material. The chemical composition formula of the rare earth doped barium ferrite is Ba1‑xLnxFe12‑xAxO19In the compound, the element Ln is rare earth elements such as La, Yb and the like, the element A is divalent transition metal elements such as Co and the like, and x is more than or equal to 0 and less than or equal to 0.5. The invention prepares Ba by coprecipitation method of Taylor reactor1‑xLnxFe12‑ xAxO19The precursor is subjected to magnetic field orientation and sintering to obtain the rare earth doped barium ferrite, the preparation method can obtain the precursor with good crystallinity and the size of 100-200nm, and the barium ferrite obtained after sintering has higher magnetic property through co-doping of rare earth elements and metal elements, and the preparation method has the advantages of high crystallinity, high strength, high heat resistance and the likeThe method can effectively reduce the high-temperature sintering temperature and time and save energy consumption.
Description
Technical Field
The invention relates to a preparation method of a high-performance nano rare earth doped barium ferrite permanent magnetic material, belonging to the field of magnetic materials.
Background
In recent years, ferrite materials have been rapidly developed, and rare earth barium ferrite materials have attracted wide attention by virtue of the advantages of uniaxial magnetic anisotropy, high coercive force, high Curie temperature, strong chemical stability, excellent cost performance and the like.
However, the ferrite material prepared by the traditional high-temperature solid-phase sintering has the disadvantages of complex process flow, long sintering time and high temperature requirement, so that the energy consumption is very high, and the prepared ferrite material has low uniformity.
In order to improve the magnetic property of ferrite materials and reduce energy consumption, researchers adopt sol-gel methods and coprecipitation methods to prepare nano-scale to micro-scale ferrite materials, and improve the magnetic property of the materials, such as the preparation methods of nano-ferrites of patents CN201210418388.8, CN201110102232.4, CN106082349A, CN201310601472.8, CN108554414A and CN108046791A, etc., but the ferrites prepared by the coprecipitation methods generally have small amount, poor repeatability and can not be produced continuously, and in addition, the sol-gel methods cause large pollution and uncontrollable appearance, so that the two methods can not be applied to actual industrial production in a large scale.
The ferrite material prepared by the Taylor reactor adopted by the invention has the advantages that the precursor particle size can be controlled between 100-200nm, the coercive force is high, the magnetic energy product is obviously improved, the ferrite precursor can be obtained by continuous production, compared with a solid-phase sintering method, the calcination temperature is lower, the use energy consumption is favorably reduced, the cost performance is improved, and the method is suitable for industrial production.
Disclosure of Invention
The invention aims to provide a method for preparing a nano high-performance rare earth doped barium ferrite permanent magnetic material by utilizing a Taylor reactor, in particular to a method for preparing Ba1-xLnxFe12-xAxO19Compared with the existing method for preparing rare earth doped barium ferrite by the traditional high-temperature solid-phase sintering method, the ferrite precursor has better uniformity and lower energy consumption.
The invention provides a preparation method of a high-performance nano rare earth doped barium ferrite permanent magnet material, which comprises the following preparation steps of (1) adding a coprecipitation solution containing rare earth elements, divalent metals, iron elements and barium elements into a Taylor reactor to prepare Ba1-xLnxFe12-xAxO19A precursor, wherein x is more than or equal to 0 and less than or equal to 0.5; (2) orienting the obtained precursor in a magnetic field, and pressing into a block-shaped or annular magnet; (3) placing the obtained block or ring magnet into a tube furnace, adding a magnetic field, and sintering at high temperature to obtain Ba1- xLnxFe12-xAxO19A ferrite; the Taylor reactor is of a specific structure, the outer cylinder is cylindrical, the material is high-strength steel, the diameter of the outer cylinder is 20cm, the thickness of the cylinder wall is 1cm, the outer cylinder is connected with the base, the thickness of the base is 4cm, the diameter of the outer cylinder is 30cm, the outer cylinder is circular, 6 holes are formed in two sides of the outer cylinder respectively, the diameter of each hole is 1cm, the distance between every two holes is 2cm, and the holes are used as a feed inlet, a sample outlet and an inlet of a PH meter;
particularly, preferably, the magnetic field orientation in the step (2) and the magnetic field high-temperature sintering in the step (3) are carried out, and the magnitude of the applied magnetic field is 1-2T;
particularly, preferably, the inner cylinder of the taylor reactor is a triangular closed structure, and the triangular closed structure is formed by connecting 3 same rectangular square sheets to form an isosceles triangular cylinder.
In particular, preferably, the inner cylinder is driven by a motor, and the rotation speed of the inner cylinder is controlled by the motor.
Particularly, preferably, the coprecipitation process control conditions in step (1) include PH, temperature, inner cylinder rotation speed, and coprecipitation solution injection rate.
In particular, the coprecipitation solution in step (1) preferably contains a rare earth metal compound such as lanthanum oxide, a salt solution such as ferric sulfate nonahydrate, cobalt nitrate hexahydrate, and barium nitrate.
In particular, preferably, the coprecipitation solution in step (1) further includes dilute nitric acid and sodium hydroxide solution.
In particular, it is preferable that the control conditions in the sintering process in the step (2) are a temperature rise rate, a sintering temperature, and a time.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) ba prepared by Taylor reactor1-xLnxFe12-xAxO19The ferrite precursor has smaller grain size, the particles are driven to move through the triangular cylinder inner cylinder, the shearing force is larger, the obtained sample particles are smaller, and the exchange coupling effect is reduced due to grain refinement, so that the coercive force and the magnetic energy product of the ferrite are effectively improved;
(2) compared with the traditional high-temperature solid-phase sintering method for preparing the ferrite material, the method has the advantages that the required calcination temperature is lower, the energy consumption is less, the sample uniformity is better, and the crystallinity is better;
(3) the ferrite obtained by orientation and sintering of the applied magnetic field has higher magnetic performance;
(4) the method has the advantages of simple process, sustainable product obtaining, high cost performance and suitability for industrial batch production.
Detailed Description
The preparation of Ba is illustrated below with reference to specific examples1-xLnxFe12-xAxO19Ferrite precursor and Ba1-xLnxFe12-xAxO19A method of forming a ferrite material.
Example 1
(1) Preparation of Ba by coprecipitation method using Taylor reactor1-xLnxFe12-xAxO19Precursor, Ln is Sm, A is Cu, wherein x =0.1, and Ba is prepared by adjusting molar concentration of nitrate0.9Sm0.1Fe11.9Cu0.1O19And (3) precursor.
Mixing Sm2O3，Cu(NO)3·6H2O, Fe(NO3)3·9H2O and Ba (NO)3)2According to a molar ratio of 0.1: 0.1: the ratio of 11.9:0.9 is prepared into 5L of metal salt solution of 2.5M, 30 to 40 percent of dilute nitric acid and 10 to 15 percent of NaOH solution, and deionized water is filled in a 1L Taylor reactor.
Dilute nitric acid is injected into a reactor, the Taylor reactor is heated to 70-90 ℃, prepared metal salt solution is injected into the reactor at the rate of 3-8 mL/min by a metering pump, and the stirring speed of an inner cylinder is within the range of900 rpm/min, stirring, injecting the prepared NaOH solution into the reactor at 4-9 mL/min, and overflowing the mixed solution from the reactor during continuous stirring and solution injection, wherein the reaction product Ba0.9Sm0.1Fe11.9Cu0.1O19The precursor overflows along with the overflow solution to remove granular Ba0.9Sm0.1Fe11.9Cu0.1O19Precursor, centrifugal washing the precipitate with deionized water, and drying in oven at 80 deg.C for 12 hr to obtain nanometer grade Ba0.9Sm0.1Fe11.9Cu0.1O19The size of the precursor is 50-100 nm.
(2) Taking a certain amount of precursor, putting the precursor into a mold, orienting under a 1T magnetic field, and pressing into a block magnet.
(3) Preparation of Ba by sintering process0.9Sm0.1Fe11.9Cu0.1O19Magnetic refrigeration material, Ba of bulk magnet0.9Sm0.1Fe11.9Cu0.1O19Putting the precursor into a tube furnace, heating at a speed of 5 ℃/min, preserving heat for 5 hours when the temperature rises to 500 ℃, preserving heat for 2 hours when the temperature rises to 800 ℃, then closing the tube furnace, naturally cooling to room temperature, and applying a 1T magnetic field on the sample in the whole sintering process to obtain Ba0.9Sm0.1Fe11.9Cu0.1O19Ferrite.
Example 2
(1) Preparation of Ba by coprecipitation method using Taylor reactor1-xLnxFe12-xAxO19Precursor, Ln is Yb, A is Ni, wherein x =0.1, Ba is prepared by adjusting molar concentration of nitrate0.9Yb0.1Fe11.9Ni0.1O19And (3) precursor.
Mixing Yb (NO)3)3·5H2O，Ni(NO3)3·6H2O，Fe(NO3)3·9H2O and Ba (NO)3)2According to a molar ratio of 0.1: 0.1: 11.9:0.9 is prepared into 2.5M of 5L metal salt solution, and 30 to 40 percent of dilute solutionNitric acid and 10% -15% NaOH solution were filled in a 1L Taylor reactor with deionized water.
Firstly, dilute nitric acid is injected into a reactor, the Taylor reactor is heated to 70-90 ℃, prepared metal salt solution is injected into the reactor at the rate of 3-8 mL/min by a metering pump, the stirring speed of an inner cylinder is 1500 rpm/min, the prepared NaOH solution is injected into the reactor at the rate of 4-9 mL/min while stirring, in the process of continuously stirring and injecting the solution, the mixed solution overflows from the reactor, and a reaction product Ba is obtained0.9Yb0.1Fe11.9Ni0.1O19The precursor overflows along with the overflow solution to remove granular Ba0.9Yb0.1Fe11.9Ni0.1O19The precursor is continuously centrifugally washed by deionized water, dried for 12 hours in an oven at 80 ℃, and a 2T magnetic field is applied to the sample in the whole sintering process to obtain the nano-grade Ba0.9Yb0.1Fe11.9Ni0.1O19The size is 30-70 nm.
(2) Taking a certain amount of precursor, putting the precursor into a mold, orienting under a 1.5T magnetic field, and pressing into a block magnet.
(3) Preparation of Ba by sintering process0.9Yb0.1Fe11.9Ni0.1O19Magnetic refrigeration material, Ba of the block magnet obtained in step (2)0.9Yb0.1Fe11.9Ni0.1O19Putting the precursor into a tube furnace, heating at a speed of 5 ℃/min, preserving heat for 5 hours when the temperature rises to 500 ℃, preserving heat for 2 hours when the temperature rises to 800 ℃, then closing the tube furnace, naturally cooling to room temperature, and applying a 1.5T magnetic field on the sample in the whole sintering process to obtain Ba0.9Yb0.1Fe11.9Ni0.1O19。
Claims (5)
1. A preparation method of a high-performance nano rare earth doped barium ferrite permanent magnetic material is characterized by comprising the following steps: (1) adding a coprecipitation solution containing rare earth elements, divalent metals, iron elements and barium elements into a Taylor reactor to prepare Ba1-xLnxFe12-xAxO19A precursor, wherein x is more than or equal to 0 and less than or equal to 0.5; (2) orienting the obtained precursor in a magnetic field, and pressing into a block-shaped or annular magnet; (3) placing the obtained block or ring magnet into a tube furnace, adding a magnetic field, and sintering at high temperature to obtain Ba1-xLnxFe12-xAxO19A ferrite; the Taylor reactor is of a specific structure, the outer cylinder is cylindrical, the material is high-strength steel, the diameter of the outer cylinder is 20cm, the thickness of the cylinder wall is 1cm, the outer cylinder is connected with the base, the thickness of the base is 4cm, the diameter of the outer cylinder is 30cm, the outer cylinder is circular, 6 holes are formed in two sides of the outer cylinder respectively, the diameter of each hole is 1cm, the distance between every two holes is 2cm, and the holes are used as a feed inlet, a sample outlet and an inlet of a PH meter;
the magnetic field orientation in the step (2) and the magnetic field high-temperature sintering in the step (3) are carried out, and the size of the added magnetic field is 1-2T;
the inner cylinder of the Taylor reactor is a triangular closed structure, and the triangular closed structure is formed by mutually connecting 3 same rectangular square sheets to form an isosceles triangular cylinder;
the inner cylinder is driven by a motor, and the rotating speed of the inner cylinder is controlled by the motor.
2. Preparation of Ba by coprecipitation method according to claim 11-xLnxFe12-xAxO19The precursor is characterized in that the control conditions of the coprecipitation process in the step (1) comprise PH, temperature, inner cylinder rotating speed and coprecipitation liquid injection rate.
3. Preparation of Ba by coprecipitation method according to claim 11-xLnxFe12-xAxO19The precursor is characterized in that the coprecipitation solution in the step (1) contains rare earth metal compounds such as lanthanum oxide and the like, ferric nitrate nonahydrate, cobalt nitrate hexahydrate, barium nitrate and other salt solutions.
4. The coprecipitation method of claim 1Prepare Ba1-xLnxFe12-xAxO19And (2) the precursor is characterized in that the coprecipitation solution in the step (1) further comprises dilute nitric acid and sodium hydroxide solution.
5. High temperature sintering according to claim 1 to obtain Ba1-xLnxFe12-xAxO19The magnetic refrigeration material is characterized in that the control conditions in the sintering process in the step (2) are temperature rise speed, sintering temperature and time.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114230329A (en) * | 2021-12-13 | 2022-03-25 | 湖南航天磁电有限责任公司 | Ferrite wave-absorbing material and preparation method thereof |
| CN114956192A (en) * | 2022-06-09 | 2022-08-30 | 合肥工业大学 | Lanthanum-cobalt co-doped barium ferrite dual-waveband wave-absorbing powder material and preparation method thereof |
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2020
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114230329A (en) * | 2021-12-13 | 2022-03-25 | 湖南航天磁电有限责任公司 | Ferrite wave-absorbing material and preparation method thereof |
| CN114956192A (en) * | 2022-06-09 | 2022-08-30 | 合肥工业大学 | Lanthanum-cobalt co-doped barium ferrite dual-waveband wave-absorbing powder material and preparation method thereof |
| CN114956192B (en) * | 2022-06-09 | 2024-02-20 | 合肥工业大学 | Lanthanum-cobalt co-doped barium ferrite dual-band wave-absorbing powder material and preparation method thereof |
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