CN110156451B - High-impedance lean-iron manganese-zinc ferrite material and preparation method thereof - Google Patents
High-impedance lean-iron manganese-zinc ferrite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the technical field of soft magnetic ferrite, and aims to solve the problems of low impedance and low magnet resistivity at high frequency in the existing EMI (electro-magnetic interference) resisting technologyThe high-impedance lean-iron manganese-zinc ferrite material is prepared from a main material and an auxiliary material, wherein the main material comprises 46.0-49.8 mol% of Fe in terms of mole percentage2O327.2-37.0 mol% MnO, 17.0-23.0 mol% ZnO; the auxiliary materials comprise the following components in percentage by mass based on the total weight of the main materials: 0.03 to 0.1wt% of Co2O3，0.005～0.05wt%SnO2，0.01～0.06wt%TiO2. The MnZn ferrite material has the magnetic conductivity mu i of 2500 +/-25% at room temperature, and has good high impedance performance in the temperature range of 25-120 ℃ when the frequency f is in the range of 1 MHz-500 MHz.
Description
Technical Field
The invention relates to the technical field of soft magnetic ferrite, in particular to a high-impedance lean iron manganese zinc ferrite material and a preparation method thereof.
Background
As electronic equipment such as computers and mobile phones have increased, electromagnetic interference (EMI) of ignition devices of scientific, medical, industrial machinery, and motor transportation equipment to electronic equipment operating in their vicinity has become an increasingly serious environmental pollution.
An effective solution to the problem of reducing or improving the resistance of electronic devices to electromagnetic pollution is to use electromagnetic compatibility (EMC) designs, in which a large amount of materials against electromagnetic interference are used. The anti-electromagnetic interference ferrite mainly utilizes an electromagnetic loss mechanism of a ferrite material to absorb a large amount of electromagnetic interference signals so as to achieve the aim of resisting electromagnetic interference, and is mainly used for fixing inductors, anti-electromagnetic interference filters, suppressors and chip inductors, which require that used components have the excellent characteristics of wide temperature range, high stability and long service life.
With the increasing development of electronic technology, especially the rapid development of digital technology. The EMI resistance of electronic equipment is very important in all countries of the world, and how to effectively reduce the electromagnetic wave interference of electronic equipment becomes a problem generally concerned by researchers. The soft magnetic ferrite is made into various components for inhibiting EMI, and the components are widely applied to various electronic equipment to prevent unnecessary signal feedback and coupling and avoid parasitic oscillation, thereby effectively inhibiting conduction and radiation noise. The existing EMI resistant technology has the problems of low impedance, low magnet resistivity, low Curie temperature and the like under high frequency, so that the EMI resistant capability of electronic equipment is limited.
Chinese patent literature discloses a manganese-zinc ferrite material and a preparation method thereof, wherein the publication number is CN104446409A, the manganese-zinc ferrite material has very low self power loss in a wide frequency range of (0.1-1) MHz, and the power loss Pcv is less than or equal to 380mW/cm under the conditions of 100kHz, 200mT and 100 ℃ through tests3(ii) a Under the conditions of 300kHz, 100mT and 100 ℃, the power loss Pcv is less than or equal to 350; the power loss Pcv is less than or equal to 5mW/cm at the temperature of 500kHz, 50mT and 100 DEG C31MHz, 30mT and 100 ℃ power loss Pcv less than or equal to 85mW/cm3(ii) a Meanwhile, the manganese-zinc ferrite material has higher Curie temperature and Tc is more than or equal to 270 ℃. However, the Mn-Zn ferrite material has low resistance and limited EMI resistance for electronic devices.
Disclosure of Invention
The invention provides a high-impedance lean iron manganese zinc ferrite material with higher magnetic permeability value and Curie temperature Tc, aiming at overcoming the problems of low impedance, low magnet resistivity and low Curie temperature under high frequency in the existing EMI resistant technology.
The invention also provides a preparation method of the high-impedance lean iron manganese zinc ferrite material, which has simple steps, has no special requirements on equipment and is easy to realize large-scale industrial production.
In order to achieve the purpose, the invention adopts the following technical scheme:
the high-impedance lean-iron manganese-zinc ferrite material is prepared from a main material and an auxiliary material, wherein the main material comprises 46.0-49.8 mol% of Fe in terms of mole percentage2O327.2-37.0 mol% MnO, 17.0-23.0 mol% ZnO; the auxiliary materials comprise the following components in percentage by mass based on the total weight of the main materials: 0.03 to 0.1wt% of Co2O3，0.005～0.05wt％SnO2，0.01～0.06wt％TiO2。
Based on the development trend and market demand, the invention develops the research on the preparation process of the ferrite material for the 1-500 MHz high-frequency EMI resistant module. The MnZn ferrite is prepared by adopting an oxide ceramic process, and the resistivity and the product impedance performance of the MnZn ferrite are improved mainly from three aspects of main materials, auxiliary materials and process conditions. The poor-iron MnZn ferrite almost has the low-frequency characteristic of the rich-iron MnZn ferrite and the high-frequency characteristic of the NiZn ferrite, and the Curie temperature Tc is not low, so that the poor-iron MnZn ferrite is a soft magnetic ferrite material with great application potential. In MnZn ferrite, Fe is designed2O3With a molar ratio of less than 50%, it is possible to suppress Fe2+Thereby increasing the grain resistivity and greatly reducing the loss of MnZn ferrite material.
The high-frequency high-impedance manganese-zinc high-permeability material is prepared by controlling Fe to obtain higher permeability value and high Curie temperature Tc2O3And ZnO content. Fe due to the high initial permeability and high impedance value2O3And the content of ZnO needs to be reasonably matched and adjusted. When Fe2O3And ZnO can satisfy the requirements of magnetic conductivity and high frequency and high impedance at the same time when the content of the Fe and ZnO is within the content range of the invention2O3When the content is less than the content range of the present invention, the initial permeability after sintering is less than 1800, and the low frequency impedance is low. When Fe2O3The high frequency impedance will be low when the content of (b) is higher than the content range of the present invention. The room temperature magnetic permeability mu i is 2000 plus or minus 25% (the testing condition f is 10kHz, and u is 0.15V), and the magnetic core has good high impedance performance in the temperature range of 25 ℃ to 120 ℃ under the condition that the frequency f is between 1MHz and 500 MHz.
The first accessory ingredient Co in the auxiliary material2O3The main functions of the method are as follows: by adding Co2O3Can generate CoFe with high K1 positive value2O4Due to Co2+Has a large K1 value, so that the composition is CoFe2O4The content of the magnetic material determines the position of the II peak of the material to a great extent, thereby the magnetic permeability and the impedance value change of 25 ℃ and 120 ℃ can be consideredAnd (4) transforming. In addition, the hysteresis coefficient has a certain corresponding relation with the magnetic permeability, the material with high magnetic permeability also has small hysteresis coefficient, the material with low opposite magnetic permeability has large hysteresis coefficient, and the magnetic permeability is in direct proportion to the reciprocal of K1, obviously, the hysteresis coefficient has an internal relation with K1, and the Fe is adjusted2+And Co2+The content of (b) makes the K1 value approach to zero, reduces the hysteresis coefficient and improves the magnetic permeability. While the subcomponent SnO2And TiO2By lowering the pre-firing temperature, the solid-phase reaction of ferrite can be promoted because of part of Sn4+And Ti4+Ion substituted Fe3+The ions enter the ferrite crystal lattice, so that the resistivity inside the ferrite crystal grains is improved; further additive TiO2The crystal grains can be uniformly grown to improve the magnetic conductivity, and the high-frequency impedance characteristic of the material can be improved.
The high-impedance lean iron manganese zinc ferrite material has the following characteristics: the magnetic permeability mu i is 2500 +/-25 percent at room temperature (the testing conditions f is 10kHz, and u is 0.25V), and the magnetic core has good high impedance performance in the temperature range of 25-120 ℃ under the condition that the frequency f is 1 MHz-500 MHz.
The invention can prepare high-impedance lean iron manganese zinc ferrite material only by strictly according to the mixture ratio (main material and auxiliary material), and particularly, the invention has to control Fe2O3In a proportion of 46.0 to 49.8 mol% Fe2O3When being Fe2O3The content of the ferrite material (iron-rich formula) is higher than 50 mol%, the 100MHz high-frequency impedance value is lower than 400 omega/cm, and the ferrite material cannot be used; this is because of the small amount of Fe in the iron-rich formulation2+Exist, form Fe in the crystal lattice2+-Fe3+Electron pair, electrons in Fe2+、Fe3+Thereby causing the resistivity of the material to drop. When Fe2O3The ferrite material obtained with the content lower than 46mol percent has a 1MHz high-frequency impedance value lower than 800 omega/cm and does not meet the requirement; when the ZnO content is not in the above proportioning range, the resistivity is high and can meet the characteristic requirements of the device, but the impedance has low performance at high frequency. The proportion of the auxiliary material is also important to the performance of the product, and when the cobalt oxide is less than 300ppm, the magnetic conductance of the obtained materialThe frequency is low, and the low-frequency impedance performance is poor; when the cobalt oxide is more than 0.1wt%, the obtained material has low magnetic permeability and poor resistance. When the tin oxide content exceeds 500ppm, the magnetic core crystal particles grow abnormally, and the performance is low, so that the magnetic core cannot be used.
A preparation method of a high-impedance lean-iron manganese-zinc ferrite material comprises the following steps:
(1) preparing materials: after the main material and the auxiliary material are weighed according to the proportion, deionized water is added into the main material for primary sanding, and spray drying is carried out to obtain a spray material;
(2) pre-burning: pre-burning the sprayed material to obtain a pre-burned material;
(3) secondary sanding: adding auxiliary materials into the pre-sintering material, and then adding deionized water for secondary sanding to obtain a secondary sanding material;
(4) spray granulation and forming: adding PVA (polyvinyl acetate) accounting for 0.04-0.12 wt% of the mass of the secondary sand grinding material and defoaming agent accounting for 0.001-0.05 wt% of the mass of the secondary sand grinding material into the secondary sand grinding material, and performing spray granulation and molding to obtain a ring blank; the defoaming agent is common defoaming agent in the field, such as emulsified silicone oil, higher alcohol fatty acid ester compound, polyoxyethylene polyoxypropylene pentaerythritol ether, polyoxyethylene polyoxypropylene amine ether, polyoxypropylene glycerol ether, polyoxypropylene polyoxyethylene glycerol ether, polydimethylsiloxane, etc.;
(5) and (3) sintering: and sintering the ring blank to obtain the high-impedance lean iron manganese zinc ferrite material.
Preferably, in the step (1), the primary sanding time is 10-30 min.
Preferably, in the step (2), the pre-sintering temperature is 750-900 ℃, and the pre-sintering time is 3-6 hours.
Preferably, in the step (2), the feeding amount is 200-300 kg/h.
Preferably, in the step (3), the secondary sanding time is 30-80 min;
preferably, in the step (3), the particle size distribution of the secondary sand abrasive is controlled in the range of X50: 1.0-1.4 μm; x99: 2.0 to 3.6 μm.
Xb ═ a μm: the grain diameter of less than a mu m accounts for b% of the total volume, X50 is a median diameter, is another expression form of average grain diameter and represents that the grains of less than 1.0-1.4 mu in the secondary sand grinding material account for 50%; x99 represents 99% of the particles smaller than 2.0-3.6 μm in the secondary sand grinding material. The large-flow eccentric disc type novel horizontal sand mill is adopted, the granularity of material slurry can reach the range quickly, the function of controlling the distribution range of the granularity is to form uniform and fine grains after subsequent sintering, and the product with uniform and stable impedance performance can be obtained.
Preferably, in the step (4), the particle size of the spray-granulated material is 50 to 200 μm.
Preferably, in the step (5), the sintering temperature variation curve is as follows: heating the mixture from room temperature to 500-600 ℃ at a heating rate of 2-3 ℃/min, and keeping the temperature for 3 hours;
continuously heating to 900-1100 ℃ at a heating rate of 3-5 ℃/min, and controlling the volume concentration of oxygen within the temperature range of 900-1100 ℃ to be 0.3-3%; in the stage, the heating rate is increased in order to enable Co ions to enter crystal grains and improve the magnetic permeability of the crystal grains; the oxygen concentration is controlled to be 0.3-3% at about 1000 ℃ so as to prevent Mn/Fe from being oxidized and generate substances with poor magnetic property;
continuously heating to 1200-1350 ℃ at the heating rate of 1.5-2.5 ℃/min, and preserving the heat at 1200-1350 ℃ for 4-6 h; the temperature rise rate is reduced at this stage because the temperature rise rate can ensure that Ti and Sn plasma enter the interior of the crystal grain at high temperature, and the high-frequency impedance performance of the crystal grain is improved; at the grain boundary, the crystal grain defects are reduced, and the grain boundary resistivity is improved;
in the cooling process, reducing the temperature from 1200-1350 ℃ to 1000 ℃ at a cooling speed of 2-3 ℃/min in vacuum; the cooling in vacuum is used for reducing the crystal grain defects;
cooling from 1000 ℃ to 150 ℃ at a cooling speed of 3-4 ℃/min, and then naturally cooling to room temperature.
Therefore, the invention has the following beneficial effects:
(1) the specific component proportion of the lean iron manganese zinc ferrite material is optimized and adjusted, the specific component types and contents of the main material and the auxiliary material are limited, and the components are synergistic, so that the magnetic permeability mu i of the MnZn ferrite material is 2500 +/-25% (under the test condition f is 10kHz, and u is 0.25V), and the magnetic core has good high impedance performance within the temperature range of 25-120 ℃ under the condition that the frequency f is 1 MHz-500 MHZ;
(2) the preparation method has simple steps and strong operability, and is suitable for industrial production.
Detailed Description
The technical solution of the present invention is further specifically described below by way of specific examples.
In the present invention, all the equipment and materials are commercially available or commonly used in the art, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1
(1) Preparing materials: according to 48 mol% Fe2O3Weighing each component as a main material according to the molar percentage of 33 mol% MnO and 19 mol% ZnO; based on the total weight of the main materials, 0.09 wt% of Co2O3，0.03wt％SnO2，0.04wt％TiO2Weighing the components as auxiliary materials according to the mass percentage; adding deionized water into the main material in a sand mill, mixing and crushing, performing primary sand milling for 30min, circularly mixing for 10min, and performing spray drying to obtain a spray material;
(2) pre-burning: pre-burning the sprayed material in a rotary kiln pre-burning furnace at 750 ℃ for 4 hours at a feeding amount of 200kg/h to obtain a pre-burned material;
(3) secondary sanding: after adding the auxiliary material in the material of presintering, add deionized water and carry out the secondary sanding, the time of secondary sanding is 80min, and the particle size distribution control of secondary sand abrasive material is at X50: 1.0 μm; x99: 3.6 mu m of the mixture with the grain size of,
obtaining secondary sand grinding materials;
(4) spray granulation and forming: adding PVA (0.04 wt% of the mass of the secondary sand grinding material) and polydimethylsiloxane serving as a defoaming agent (0.001 wt% of the mass of the secondary sand grinding material) into the secondary sand grinding material, performing spray granulation, wherein the particle size of the spray-granulated material is 50 mu m, and respectively forming the spray-granulated material into granules with the density of 3.00g/cm3H25 x 15 x 8mm standard ring blanks and cylinders
A sample;
(5) and (3) sintering: sintering the ring blank and the cylindrical sample, wherein the maximum sintering temperature range is 1200 ℃; the sintering curve is: heating from room temperature to 500 ℃ at the heating rate of 2 ℃/min, and keeping the temperature for 3 h; continuously heating to 900 ℃ at the heating rate of 3 ℃/min, and controlling the oxygen concentration to be 0.3% within the temperature range of 900 ℃; continuously heating to the highest sintering temperature at the heating rate of 1.5 ℃/min, and keeping the temperature at the highest sintering temperature for 4 h; in the cooling process, the temperature is reduced from the highest sintering temperature to 1000 ℃ in vacuum at the cooling speed of 2 ℃/min; cooling from 1000 ℃ to 150 ℃ at a cooling speed of 3 ℃/min, and then naturally cooling to room temperature to obtain the high-impedance lean iron manganese zinc ferrite material;
(6) and (3) testing: testing and evaluating the sintered magnetic ring: under the condition that the number of turns N is 20Ts, an LCR tester of E4991A type is used for testing the initial permeability mu i and the impedance value of the magnetic ring sample; the saturated magnetic induction Bs (1KHz/1200A/m) of the sample was measured by a SY-8258 type B-H analyzer, and the Curie temperature Tc of the sample was measured by an LCR-4225 type induction analyzer and a special oven. The insulation resistance values R at the two ends Φ 4 × 5 were measured by a digital multimeter DT4252, and the resistivity ρ was calculated, and the measurement results were recorded in table 1.
Examples 2 to 5
Examples 2-5 differ from example 1 in the main material, as shown in table 1, and the preparation process and test conditions were exactly the same as in example 1.
Comparative examples 1 to 4
Comparative examples 1 to 4 are different from example 1 in that the main material is different, and specifically, see table 1, the preparation process and the test conditions are completely the same as those of example 1.
TABLE 1 Main Material formulation and Performance test Table for examples 1-5 and comparative examples 1-4
As can be seen from Table 1, Fe in comparative example 12O3The ferrite material obtained with the content higher than 50mol percent has the high-frequency impedance value of 100MHz lower than400 omega/cm, cannot be used; this is because of the small amount of Fe in the iron-rich formulation2+Exist, form Fe in the crystal lattice2+-Fe3+Electron pair, electrons in Fe2+、Fe3+Thereby causing the resistivity of the material to drop. Fe in comparative example 22O3The ferrite material obtained with the content lower than 46mol percent has a 1MHz high-frequency impedance value lower than 800 omega/cm and does not meet the requirement; it can be seen from the performance data of comparative example 3 that, when the ZnO content is not the component requirement content, the resistivity is high and can satisfy the characteristic requirement of the device, but the impedance has a low performance at a high frequency.
Example 6
(1) Preparing materials: 46 mol% Fe2O3Weighing each component as a main material according to the molar percentage of 34 mol% MnO and 20 mol% ZnO; based on the total weight of the main materials, the weight percentage of Co is 0.082O3，0.02wt％SnO2，0.03wt％TiO2Weighing the components as auxiliary materials according to the mass percentage; adding deionized water into the main material in a sand mill, mixing and crushing, performing primary sand milling for 10min, circularly mixing for 15min, and performing spray drying to obtain a spray material;
(2) pre-burning: pre-burning the sprayed material in a rotary kiln pre-burning furnace at 900 ℃ for 3 hours at a feeding amount of 300kg/h to obtain a pre-burned material;
(3) secondary sanding: after adding the auxiliary material in the material of presintering, add deionized water and carry out the secondary sanding, the time of secondary sanding is 30min, and the particle size distribution control of secondary sand abrasive material is at X50: 1.4 μm; x99: 2.0 μm to obtain secondary sand abrasive;
(4) spray granulation and forming: adding PVA (0.12 wt% of the mass of the secondary sand grinding material) and polydimethylsiloxane serving as a defoaming agent in an amount of 0.05wt% into the secondary sand grinding material, performing spray granulation, wherein the particle size of the spray granulated material is 200 mu m, and respectively forming the spray granulated material into granules with the density of 3.15g/cm3H25 x 15 x 8mm standard ring blanks and cylinders
A sample;
(5) and (3) sintering: sintering the ring blank and the cylindrical sample, wherein the maximum sintering temperature range is 1350 ℃; the sintering curve is: heating from room temperature to 600 ℃ at the heating rate of 3 ℃/min, and keeping the temperature for 3 h; continuously heating to 1100 ℃ at the heating rate of 5 ℃/min, and controlling the oxygen concentration within the temperature range of 1100 ℃ to be 3%; continuously heating to the highest sintering temperature at the heating rate of 2.5 ℃/min, and keeping the temperature at the highest sintering temperature for 6 hours; in the cooling process, the temperature is reduced from the highest sintering temperature to 1000 ℃ in vacuum at the cooling speed of 3 ℃/min; cooling from 1000 ℃ to 150 ℃ at a cooling rate of 4 ℃/min, and then naturally cooling to room temperature to obtain the high-impedance lean iron manganese zinc ferrite material;
(6) and (3) testing: testing and evaluating the sintered magnetic ring: under the condition that the number of turns N is 20Ts, an LCR tester of E4991A type is used for testing the initial permeability mu i and the impedance value of the magnetic ring sample; the saturated magnetic induction Bs (1KHz/1200A/m) of the sample was measured by a SY-8258 type B-H analyzer, and the Curie temperature Tc of the sample was measured by an LCR-4225 type induction analyzer and a special oven. The insulation resistance values R at the two ends Φ 4 × 5 were measured by a digital multimeter DT4252, and the resistivity ρ was calculated, and the measurement results were recorded in table 2.
Examples 7 to 10
Examples 7 to 10 differ from example 6 in the difference of the auxiliary materials, and specifically, see table 2, the preparation process and the test conditions were exactly the same as example 6.
Comparative examples 5 to 9
Comparative examples 5 to 9 differ from example 6 in the difference of the auxiliary materials, and specifically, see table 2, the preparation process and the test conditions were exactly the same as example 6.
TABLE 2 formulation of adjuvants and Performance test Table for examples 6-10 and comparative examples 5-9
As can be seen from Table 2, the cobalt oxide added in comparative example 7 is less than 300ppm, and the obtained material has low magnetic permeability and poor low-frequency impedance performance; comparative example 8 added tin oxide more than 500ppm, abnormal growth of magnetic core crystal particles, low performance, unable to use; when the cobalt oxide added in comparative example 9 exceeds 0.1wt%, the obtained material has low magnetic permeability and poor resistance.
From a comparison of the properties of the examples of tables 1 and 2: the magnetic permeability mu i of the soft magnetic material is 2500 +/-25% at room temperature (under the test condition f, 10kHz, u and 0.25V), and the magnetic core has good high impedance performance under the condition that the frequency f is 1-500 MHz.
Therefore, the soft magnetic ferrite material has the characteristics of high frequency, high impedance and high resistivity, and has a very good market prospect in the aspect of EMI resistance.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (5)
1. The high-impedance lean-iron manganese-zinc ferrite material is prepared from a main material and an auxiliary material, and is characterized in that the main material comprises 46.0-49.8 mol% of Fe in terms of mole percentage2O327.2-37.0 mol% MnO, 17.0-23.0 mol% ZnO; the auxiliary materials comprise the following components in percentage by mass based on the total weight of the main materials: 0.03 to 0.1wt% of Co2O3，0.005~0.02wt%SnO2，0.02～0.06wt%TiO2；
The preparation method of the high-impedance lean-iron manganese-zinc ferrite material comprises the following steps:
(1) preparing materials: after the main material and the auxiliary material are weighed according to the proportion, deionized water is added into the main material for primary sanding, and spray drying is carried out to obtain a spray material;
(2) pre-burning: pre-burning the sprayed material to obtain a pre-burned material; the pre-sintering temperature is 750-900 ℃, and the pre-sintering time is 3-6 hours;
(3) secondary sanding: adding auxiliary materials into the pre-sintering material, and then adding deionized water for secondary sanding to obtain a secondary sanding material; the particle size distribution of the secondary sand abrasive is controlled to be X50: 1.0-1.4 μm; x99: 2.0-3.6 μm;
(4) spray granulation and forming: adding PVA (polyvinyl acetate) accounting for 0.04-0.12 wt% of the mass of the secondary sand grinding material and defoaming agent accounting for 0.001-0.05 wt% of the mass of the secondary sand grinding material into the secondary sand grinding material, and performing spray granulation and molding to obtain a ring blank; the particle size of the spray granulated material is 50-200 mu m;
(5) and (3) sintering: sintering the ring blank to obtain a high-impedance lean iron manganese zinc ferrite material; the sintering temperature change curve is as follows: heating the mixture from room temperature to 500-600 ℃ at a heating rate of 2-3 ℃/min, and keeping the temperature for 3 hours; continuously heating to 900-1100 ℃ at a heating rate of 3-5 ℃/min, and controlling the volume concentration of oxygen within the temperature range of 900-1100 ℃ to be 0.3-3%; continuously heating to 1200-1350 ℃ at the heating rate of 1.5-2.5 ℃/min, and preserving the heat at 1200-1350 ℃ for 4-6 h; in the cooling process, reducing the temperature from 1200-1350 ℃ to 1000 ℃ at a cooling speed of 2-3 ℃/min in vacuum; cooling from 1000 ℃ to 150 ℃ at a cooling speed of 3-4 ℃/min, and then naturally cooling to room temperature.
2. A method of making a high impedance iron-depleted manganese-zinc ferrite material of claim 1, comprising the steps of:
(1) preparing materials: after the main material and the auxiliary material are weighed according to the proportion, deionized water is added into the main material for primary sanding, and spray drying is carried out to obtain a spray material;
(2) pre-burning: pre-burning the sprayed material to obtain a pre-burned material; the pre-sintering temperature is 750-900 ℃, and the pre-sintering time is 3-6 hours;
(3) secondary sanding: adding auxiliary materials into the pre-sintering material, and then adding deionized water for secondary sanding to obtain a secondary sanding material; the particle size distribution of the secondary sand abrasive is controlled to be X50: 1.0-1.4 μm; x99: 2.0-3.6 μm;
(4) spray granulation and forming: adding PVA (polyvinyl acetate) accounting for 0.04-0.12 wt% of the mass of the secondary sand grinding material and defoaming agent accounting for 0.001-0.05 wt% of the mass of the secondary sand grinding material into the secondary sand grinding material, and performing spray granulation and molding to obtain a ring blank; the particle size of the spray granulated material is 50-200 mu m;
(5) and (3) sintering: sintering the ring blank to obtain a high-impedance lean iron manganese zinc ferrite material; the sintering temperature change curve is as follows: heating the mixture from room temperature to 500-600 ℃ at a heating rate of 2-3 ℃/min, and keeping the temperature for 3 hours; continuously heating to 900-1100 ℃ at a heating rate of 3-5 ℃/min, and controlling the volume concentration of oxygen within the temperature range of 900-1100 ℃ to be 0.3-3%; continuously heating to 1200-1350 ℃ at the heating rate of 1.5-2.5 ℃/min, and preserving the heat at 1200-1350 ℃ for 4-6 h; in the cooling process, reducing the temperature from 1200-1350 ℃ to 1000 ℃ at a cooling speed of 2-3 ℃/min in vacuum; cooling from 1000 ℃ to 150 ℃ at a cooling speed of 3-4 ℃/min, and then naturally cooling to room temperature.
3. The preparation method of the high-impedance lean-iron manganese-zinc ferrite material according to claim 2, wherein in the step (1), the primary sanding time is 10-30 min.
4. The preparation method of the high-impedance lean-iron manganese-zinc ferrite material according to claim 2, wherein in the step (2), the feeding amount is 200-300 kg/h.
5. The preparation method of the high-impedance lean-iron manganese-zinc ferrite material according to claim 2, wherein in the step (3), the secondary sanding time is 30-80 min.
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| CN111138180A (en) * | 2019-12-25 | 2020-05-12 | 江门安磁电子有限公司 | Broadband high-impedance manganese-zinc ferrite material and preparation method thereof |
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