CN115894006A - Preparation method of ferrite material with high frequency, high Bs and low loss power - Google Patents

Preparation method of ferrite material with high frequency, high Bs and low loss power Download PDF

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CN115894006A
CN115894006A CN202211722230.XA CN202211722230A CN115894006A CN 115894006 A CN115894006 A CN 115894006A CN 202211722230 A CN202211722230 A CN 202211722230A CN 115894006 A CN115894006 A CN 115894006A
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sanding
drying
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郭文强
吕海波
高喜英
刘娜
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Beijing Seven Star Flight Electronic Co ltd
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Abstract

The invention relates to a preparation method of a ferrite material with high frequency, high Bs and low loss power. The ferrite material comprises a main component and an auxiliary agent, wherein the main component comprises Fe in mol percentage 2 O 3 56-58%, mnO 39-42%, znO 3-5%; the adjuvant comprises Co 2 O 3 And TiO 2 2 Wherein, co 2 O 3 The dosage of the main component is 0.4 to 0.6 percent of the total weight of the main component, and the TiO 2 The dosage of the main component is 0.2 to 0.35 percent of the total weight of the main component. The preparation method of the invention reduces the proportion of hysteresis loss in total loss and improves the loss performance of ferrite under high magnetic field strength value; addition of Co 2 O 3 And TiO 2 As an auxiliary agent, the permeability curve of the material is smoothed, the high-temperature permeability is reduced, and the reduction of the permeability is avoidedAt high temperatures the permeability is too high, resulting in a shift of the domain resonance frequency to low frequencies resulting in a sharp increase in residual losses.

Description

Preparation method of ferrite material with high frequency, high Bs and low loss power
Technical Field
The invention relates to a preparation method of a ferrite material with high frequency, high Bs and low loss power, belonging to the technical field of magnetic material production.
Background
Currently, as a magnetic material most used in devices such as power transformers, mn — Zn-based ferrite materials have high magnetic permeability and low loss in a low frequency region of about 100kHz, and satisfy important characteristics as a magnetic core material. However, when the ferrite material is operated at a drive frequency of several MHz, the loss is significantly increased, the power loss is low, and the device is difficult to be used and is difficult to satisfy the application.
The prior art ferrites are typically in the form of Fe 2 O 3 MnO and ZnO are used as raw materials, and a plurality of auxiliary agents are added to achieve the conditions of high magnetic conductivity and high saturation magnetic induction intensity. However, in the prior art, the loss mechanism of the ferrite is changed under high-frequency and high-magnetic-field strength, and the lowest loss point moves forward, so that the rise amplitude of loss at high temperature is large. The loss of the magnetic core is large, which not only causes the energy consumption to be greatly increased, but also is not beneficial to the working characteristics of the magnetic core, so that the ferrite magnetic core with high frequency and high Bs in the prior art can not meet the use requirements under the high temperature condition.
Disclosure of Invention
Technical problem to be solved
In order to solve the above problems in the prior art, the present invention provides a method for preparing a ferrite material with high frequency, high Bs and low loss.
(II) technical scheme
In order to achieve the purpose, the invention adopts the main technical scheme that:
the ferrite material with high frequency, high Bs and low loss power comprises a main component and an auxiliary agent, wherein the main component comprises Fe in mole percentage 2 O 3 56-58%, mnO 39-42%, znO 3-5%; the adjuvant comprises Co 2 O 3 And TiO 2 2 Wherein, co 2 O 3 The dosage of the main component is 0.4 to 0.6 percent of the total weight of the main component, and the TiO 2 The dosage of the main component is 0.2 to 0.35 percent of the total weight of the main component.
A preparation method of the ferrite material with high frequency, high Bs and low loss power comprises the following steps:
s1, weighing main components in proportion, carrying out wet mixing and sanding on the main components, and then carrying out primary drying to obtain a primary sanding material;
s2, pre-burning the primary sand grinding material to obtain a pre-burned material;
s3, adding an auxiliary agent into the pre-sintered material, performing wet sanding again, and drying to obtain a secondary sanding material;
s4, adding a binder into the secondary sand grinding material, granulating, and then pressing and molding the granules to obtain a blank;
and S5, sintering the blank to obtain the ferrite material.
The preparation method as described above, preferably, in step S1, the sand milling, material mixing: ball: the mass ratio of water is 1: 4.5-6: 1-3, the rotating speed of the ball mill is 60-80 r/min, and the sanding time is 40-70 min; the temperature of the primary drying is 110-120 ℃, and the time of the primary drying is 15-20 h.
In the above-mentioned preparation method, preferably, in step S2, the temperature is raised to 920-940 ℃ at a temperature raising rate of 2-3 ℃/min during the pre-sintering, and the pre-sintering time is 2-3 h.
In the above-described production method, preferably, in step S3, the material used for wet sanding is again: ball: water is mixed according to the mass ratio of 1: 4.5-6: 1-3, the rotating speed of the ball mill is 35-45 r/min, and the sanding time is 90-120 min; the drying temperature is 110-120 ℃, and the drying time is 15-25 min.
In the preparation method, in step S4, the binder is polyvinyl alcohol, the binder is an aqueous solution with a mass concentration of 7.5 to 10.5%, and the amount of the binder is 2.3 to 4% of the mass of the regrind material.
In the preparation method, in step S5, the sintering temperature is 1200-1250 ℃, the sintering time is 4-5 h, the sintering time is too short, the sintering is insufficient, the sintering time is too long, and the energy consumption is too high, and the sintering time is preferably 4-5 h.
In the production method described above, in step S5, the blank is sintered under the condition that the oxygen partial pressure is controlled to be 4 to 6 vol%.
(III) advantageous effects
The beneficial effects of the invention are:
the preparation method of the ferrite material with high frequency, high Bs and low loss provided by the invention optimizes the raw material composition and the dosage thereof, and properly reduces Fe 2+ Content, the hysteresis loss valley bottom is moved to high temperature; the proportion of hysteresis loss in total loss is reduced, and the loss performance of the ferrite under a high magnetic field strength value is improved; addition of Co 2 O 3 And TiO 2 As an auxiliary agent, the magnetic permeability curve of the material is smoothed, the high-temperature magnetic permeability is reduced, and the situation that the residual loss is increased sharply due to the fact that the magnetic domain resonance frequency moves to a low frequency at a high temperature is avoided.
Detailed Description
The invention provides
For a better understanding of the present invention, reference will now be made in detail to the present invention by way of specific embodiments thereof.
Example 1
A high frequency, high Bs, low loss power ferrite material comprising the steps of:
s1, weighing the main component Fe according to the mole percentage 2 O 3 57%, mnO 40%, znO 3%; carry out wet-type mixing and sanding to the principal ingredients raw materials, wherein, material: ball: water is mixed according to the mass ratio of 1:5:2, the rotating speed of the ball mill is 70 r/min, and the sanding time is 60min; then, carrying out primary drying at the drying temperature of 110 ℃, and drying for 20 hours to obtain a primary grinding material;
s2, heating the primary sand grinding material to 930 ℃ at a heating rate of 2 ℃/min, and presintering for 2.5 hours to obtain a presintering material;
s3, adding an auxiliary agent Co into the pre-sintering material 2 O 3 And TiO 2 2 ,Co 2 O 3 The dosage of the active ingredient is 0.5 percent of the total weight of the main ingredient, and the TiO is 2 Is 0.3% of the total weight of the main components, and then is subjected to wet sanding again, wherein: ball: water is mixed according to the mass ratio of 1:5:2, the rotating speed of the ball mill is 40 r/min, and the sanding time is 100min; then drying, namely bakingDrying at 120 deg.C for 10min to obtain secondary grinding material;
s4, adding a polyvinyl alcohol aqueous solution (mass concentration is 8%) into the regrind material, wherein the dosage of polyvinyl alcohol is 2.5% of the mass of the regrind material, and performing compression molding on the particles after granulation to obtain a blank;
and S5, sintering the blank at 1230 ℃ for 4.5h under the condition of controlling the oxygen partial pressure to be 5vol%, and cooling to room temperature to obtain the ferrite material with high frequency, high Bs and low loss power.
Example 2
A high-frequency, high-Bs, low-loss power ferrite material, comprising the steps of:
s1, weighing a main component Fe according to the mole percentage 2 O 3 56.5 percent, mnO 39 percent and ZnO4.5 percent; carry out wet-type mixing and sanding to the principal ingredients raw materials, wherein, material: ball: the mass ratio of water is 1:5:2, the rotating speed of the ball mill is 75 revolutions per minute, and the sanding time is 50min; then, carrying out primary drying at the drying temperature of 120 ℃, and drying for 15h to obtain a primary grinding material;
s2, heating the primary sand grinding material to 920 ℃ at the heating rate of 2 ℃/min, and presintering for 3 hours to obtain a presintering material;
s3, adding an auxiliary agent Co into the pre-sintering material 2 O 3 And TiO 2 ,Co 2 O 3 The dosage of the main component is 0.45 percent of the total weight of the main component, and TiO 2 Is 0.26% of the total weight of the main components, and then wet-sanding again, wherein: ball: water is mixed according to the mass ratio of 1:5:2, the rotating speed of the ball mill is 45 r/min, and the sanding time is 90min; then, drying is carried out, wherein the drying temperature is 115 ℃, and the drying time is 15min, so as to obtain the regrind material;
s4, adding a polyvinyl alcohol aqueous solution (mass concentration is 8%) into the regrind material, wherein the dosage of polyvinyl alcohol is 2.5% of the mass of the regrind material, and performing compression molding on the particles after granulation to obtain a blank;
and S5, sintering the blank at 1220 ℃ for 5h under the condition of controlling the oxygen partial pressure to be 5vol%, and cooling to room temperature to obtain the ferrite material with high frequency, high Bs and low loss.
Example 3
A high frequency, high Bs, low loss power ferrite material comprising the steps of:
s1, weighing the main component Fe according to the mole percentage 2 O 3 56%, mnO 40%, znO 3%; carry out wet-type mixing and sanding to the principal ingredients raw materials, wherein, material: ball: water is mixed according to the mass ratio of 1:5:2, the rotating speed of the ball mill is 80 revolutions per minute, and the sanding time is 50min; then, primary drying is carried out at the drying temperature of 115 ℃, and primary grinding materials are obtained after drying for 17 hours;
s2, heating the primary sand grinding material to 950 ℃ at a heating rate of 2 ℃/min, and presintering for 2 hours to obtain a presintering material;
s3, adding an auxiliary agent Co into the pre-sintering material 2 O 3 And TiO 2 ,Co 2 O 3 The dosage of the active ingredient is 0.6 percent of the total weight of the main ingredient, and the TiO is 2 Is 0.25% of the total weight of the main components, and then wet sanding is performed again, wherein: ball: the mass ratio of water is 1:5:2, the rotating speed of the ball mill is 35 r/min, and the sanding time is 120min; then drying is carried out, the drying temperature is 120 ℃, and after the drying time is 15min, the secondary sand grinding material is obtained;
s4, adding a polyvinyl alcohol aqueous solution (the mass concentration is 8.5%) into the regrind material, wherein the dosage of polyvinyl alcohol is 3% of the mass of the regrind material, and performing compression molding on the particles after granulation to obtain blanks;
and S5, sintering the blank at 1250 ℃ for 4 hours under the condition of controlling the oxygen partial pressure to be 5vol%, and cooling to room temperature to obtain the high-frequency high-Bs low-loss power ferrite material.
Comparative example 1
Based on example 1, with the difference that the amount of the main component, in particular Fe, is different 2 O 3 54%,MnO 43%,ZnO 3%。
Comparative example 2
The process was carried out on the basis of example 3, with the difference that the sintering temperature was 1300 ℃ and the sintering time was 5h.
The ferrite materials prepared in the above examples and comparative examples were tested for their properties, and the results are shown in table 1.
TABLE 1 results of performance test of materials in examples and comparative examples
Figure BDA0004028707070000051
Figure BDA0004028707070000061
As seen from the above table, the ferrite materials obtained by the method of the present invention in examples 1 to 3 are significantly superior to those in comparative examples 1 to 2 in terms of power loss and magnetic induction.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in other forms, and any person skilled in the art can change or modify the technical content disclosed above into an equivalent embodiment with equivalent changes. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.

Claims (8)

1. The ferrite material with high frequency, high Bs and low loss is characterized in that the material comprises a main component and an auxiliary agent, wherein the main component comprises Fe in mol percentage 2 O 3 56-58%, mnO 39-42%, znO 3-5%; the adjuvant comprises Co 2 O 3 And TiO 2 Wherein, co 2 O 3 The dosage of the main component is 0.4 to 0.6 percent of the total weight of the main component, and the TiO 2 The dosage of the main component is 0.2 to 0.35 percent of the total weight of the main component.
2. The method of claim 1, wherein the method comprises the steps of:
s1, weighing main components in proportion, carrying out wet mixing and sanding on the main components, and then drying the main components for the first time to obtain a primary sanding material;
s2, pre-burning the primary grinding material to obtain a pre-burnt material;
s3, adding an auxiliary agent into the pre-sintered material, performing wet sanding again, and drying to obtain a secondary sanding material;
s4, adding a binder into the secondary sand grinding material, granulating, and carrying out compression molding on the granules to obtain a blank;
and S5, sintering the blank to obtain the ferrite material.
3. The method of claim 2, wherein in step S1, the sand is sanded, as materials: ball: the mass ratio of water is 1: 4.5-6: 1-3, the rotating speed of the ball mill is 60-80 r/min, and the sanding time is 40-70 min; the temperature of the primary drying is 110-120 ℃, and the time of the primary drying is 15-20 h.
4. The method according to claim 2, wherein in step S2, the temperature is raised to 920 to 940 ℃ at a temperature raising rate of 2 to 3 ℃/min during the pre-firing, and the pre-firing time is 2 to 3 hours.
5. The method of claim 2, wherein in step S3, the material used for the wet sanding is again: ball: the mass ratio of water is 1: 4.5-6: 1-3, the rotating speed of the ball mill is 35-45 r/min, and the sanding time is 90-120 min; the drying temperature is 110-120 ℃, and the drying time is 15-25 min.
6. The method according to claim 2, wherein in step S4, the binder is polyvinyl alcohol, the binder is an aqueous solution having a mass concentration of 7.5 to 10.5%, and the amount of the binder is 2.3 to 4% by mass of the regrind material.
7. The method according to claim 2, wherein the sintering temperature is 1200 to 1250 ℃ and the sintering time is 4 to 5 hours in step S5.
8. The production method according to claim 2, wherein in step S5, the blank is subjected to sintering under a condition that the oxygen partial pressure is controlled to 4 to 6 vol%.
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