CN114085077A - High-frequency low-loss manganese-zinc ferrite for fine adjustment of ferrous ions and preparation method thereof - Google Patents

High-frequency low-loss manganese-zinc ferrite for fine adjustment of ferrous ions and preparation method thereof Download PDF

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CN114085077A
CN114085077A CN202111607712.6A CN202111607712A CN114085077A CN 114085077 A CN114085077 A CN 114085077A CN 202111607712 A CN202111607712 A CN 202111607712A CN 114085077 A CN114085077 A CN 114085077A
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frequency low
sintering
zinc ferrite
ions
loss
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CN114085077B (en
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徐涛
聂建文
张强原
张志新
邢冰冰
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Tiantong Kaili Technology Co ltd
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Abstract

The invention discloses a high-frequency low-loss manganese-zinc ferrite for fine adjustment of ferrous ions and a preparation method thereof2O3Y-X mol% (55 is less than or equal to 60), ZnO is less than 5 mol%, MgO is X mol% (X is less than or equal to 0.4), and the rest is MnO. The preparation method of the material comprises the following process steps: preparing materials; sanding and assisting with ultrasonic dispersion; pre-burning, and quickly cooling after pre-burning; sanding and assisting with ultrasonic dispersion; granulating and forming; sintering, and rapidly cooling after sintering. The ferrite main formula adopts trace Mg ions to replace Fe ionsAnd the ferrous ions are finely adjusted by using divalent Mg ions to promote the Fe ions to be biased to be trivalent through charge balance, so that the soft magnetic ferrite material realizes the low loss characteristic under high frequency, and has larger loss reduction range especially under high frequency and high temperature.

Description

High-frequency low-loss manganese-zinc ferrite for fine adjustment of ferrous ions and preparation method thereof
Technical Field
The invention relates to a manganese-zinc ferrite material and a preparation method thereof, in particular to a high-frequency low-loss manganese-zinc ferrite material for fine adjustment of ferrous ions and a preparation method thereof.
Background
With the development of miniaturization of electronic products and the increasing demand for energy conservation and emission reduction, the soft magnetic ferrite material on the electronic products is inevitably developed in the high-frequency direction. It is well known that the loss of a ferrite material is mainly composed of three components of hysteresis loss, eddy current loss and residual loss. At low frequencies, hysteresis losses dominate, and the higher the frequency, the higher the proportion of eddy current losses and residual losses. And excessive ferrous ions after sintering can obviously reduce the resistivity of the material and increase the eddy current loss and residual loss at high frequency. At present, the scientific research and business circles mainly adjust ferrous ions in the material by controlling oxygen partial pressure in the secondary doping and sintering processes, so that the loss of the high-frequency material is reduced.
In devices such as switching power supplies, ferrite needs to operate under conditions of high temperature, high frequency and high direct current superposition, so that high temperature and high saturation magnetic flux density are an important development direction of high-frequency ferrite materials. The adoption of the iron-rich formula is one of the important methods for improving the saturation magnetic flux density of the ferrite. In iron-rich formulations, the ferrous ion after sintering inevitably increases, thus increasing the total loss at high frequencies, especially at high temperatures. However, in the case of the iron-rich formula, it is difficult to adjust the ferrous ions by secondary doping and sintering process control. Firstly, in the process of pre-sintering, ferrite is basically in phase, and the elements of secondary doping are mostly high-valence and variable-valence elements at present, so that ferrous ions are not easy to adjust through material charge balance. In addition, the control of the sintering process is greatly influenced by environment, equipment and the like, and fluctuation is easily caused. Therefore, there is a need for an alternative method to control the ferrous ions in the material to a suitable level to reduce losses.
Patent document No. CN113436823A discloses a ferrite sintered magnet containing Mg in an amount of 0.01 to 0.09 mass% in order to increase Br, no mention is made of regulation of ferrous ions, and its system does not belong to manganese zinc ferrite. The influence of a small amount of iron deficiency on the performance of Mg-Mn-Zn ferrite is disclosed in journal literature (rare metal materials and engineering, 2008, 37(A01):4.) the preparation method of the Mg-Mn-Zn ferrite with a small amount of iron deficiency belongs to a sol-gel method, and Mg does not replace Fe, namely the Mg doping amount is not equal to the iron deficiency amount.
Disclosure of Invention
The invention provides a high-frequency low-loss manganese-zinc ferrite for fine adjustment of ferrous ions and a preparation method thereof, aiming at overcoming the defects of the existing method.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a high-frequency low-loss manganese-zinc ferrite material for finely adjusting ferrous ions comprises a quaternary system as a main component, and adopts an iron-rich formula, wherein the four components respectively comprise Fe2O3, Y-X mol% (Y is more than or equal to 55 and less than or equal to 60), ZnO is less than 5 mol%, MgO is X mol% (X is less than or equal to 0.4), and the balance is MnO; the minor component is a conventional dopant in the field of manganese-zinc ferrite. Compared with the conventional MnZn ferrite, the ferrite adopts trace Mg ions to replace Fe ions in the main formula, and is matched with a corresponding preparation process to avoid the precipitation of a magnesium-rich impurity phase, and divalent Mg ions are utilized to promote the Fe ions to be biased to be trivalent through charge balance, so that the aim of fine adjustment of ferrous ions is fulfilled.
The preparation method of the high-frequency low-loss manganese-zinc ferrite material for fine adjustment of ferrous ions comprises the following steps:
(1) preparing materials: weighing Fe2O3, ZnO, MgO and MnO according to a quaternary system formula, carrying out sand milling and mixing for 10-20 min, and simultaneously, in order to uniformly mix Mg, enabling the Mg to uniformly enter crystal lattices in a pre-sintering process, and carrying out ultrasonic dispersion for 3-15 min while carrying out sand milling;
(2) pre-burning: pre-burning the powder in the last step at 800-1000 ℃, keeping the temperature for 1-3 h to prevent Mg from being separated out of crystal lattices in the cooling process due to the larger radius of Mg ions, immediately transferring the powder to the environment of 25 ℃ after the heat preservation is finished, and cooling to room temperature;
(3) sanding: adding the auxiliary components into the pre-sintered material treated in the previous step, then performing sanding and mixing until the target particle size is reached, wherein D50 is 0.8-1.8 mu m, and performing ultrasonic dispersion for 3-15 min while sanding;
(4) granulating and forming;
(5) and (3) sintering: and (2) sintering the formed blank in a balanced oxygen partial pressure at the sintering temperature of 1100-1300 ℃ for 3-5 h, wherein in order to prevent Mg from being separated out from crystal lattices in the cooling process, a fast cooling rate is adopted in the cooling stage, and the cooling rate is 2-6 ℃/min below 1100 ℃.
Preferably, the material formula of the high-frequency low-loss manganese-zinc ferrite material for finely adjusting ferrous ions is Fe2O3, Y-X mol% (Y is more than or equal to 55 and less than or equal to 57), ZnO is less than 5 mol%, MgO is X mol% (X is more than or equal to 0.1 and less than or equal to 0.3), and the balance is MnO.
Preferably, in the step 2, the pre-sintering temperature is 850-950 ℃, and the heat preservation is carried out for 1-3 h.
Preferably, in the step 5, the cooling rate of the cooling stage below 1100 ℃ is between 3 ℃/min and 5 ℃/min.
Preferably, the material subcomponents of the high-frequency low-loss manganese-zinc ferrite material for finely adjusting ferrous ions can be one or more of Co2O3, TiO2, CaCO3, ZrO2, V2O5, Ta2O5, Nb2O5, CuO and SnO2, and the content ranges are Co2O 3: 0-0.8wt%, TiO 2: 0-1wt%, CaCO 3: 0.01-0.2wt%, ZrO 2: 0-0.02wt%, V2O 5: 0.01 to 0.05wt%, Ta2O 5: 0.01-0.05wt%, Nb2O 5: 0.01 to 0.03wt%, CuO: 0-0.02wt%, SnO 2: 0 to 0.02wt%, the above subcomponents being calculated by weight percentage with respect to the total amount of the main component.
The preparation method has the beneficial effects that on the basis of a quaternary system formula, a trace amount of Mg replaces Fe, and the processes of pre-sintering, sanding and sintering are matched, so that sanding and mixing are more uniform by ultrasonic, the formation of a homogeneous phase in a heat treatment process is promoted, magnesium entering crystal lattices at high temperature can be fixed in the crystal lattices by the rapid cooling of the pre-sintering and the sintering, the precipitation of magnesium-rich impurity phases is reduced, the loss at high frequency and high Bm, especially the loss at high temperature, is favorably reduced, the power consumption (25 ℃) of the prepared high-frequency ferrite magnetic core at 3MHz and 50mT is less than 700 kW/m3, the power consumption (100 ℃) of the prepared high-frequency ferrite magnetic core at 3MHz and 50mT is less than 700 kW/m3, and the low power consumption of the soft ferrite material can be kept at the high temperature of high frequency and high Bm.
Detailed Description
Example 1: a high-frequency low-loss Mn-Zn ferrite material for fine tuning ferrous ions is composed of main component and auxiliary componentAre each Fe2O356mol percent, 4mol percent of ZnO, 0.1mol percent of MgO and 39.9mol percent of MnO; the accessory ingredient is Co2O3、TiO2、CaCO3、ZrO2、V2O5、Ta2O5、Nb2O5、CuO、SnO2All examples and comparative examples are the same accessory ingredient.
The preparation method comprises the following steps:
1) preparing materials: weighing Fe according to quaternary system formula2O3ZnO, MgO and MnO, then sanding for 15min, and performing auxiliary ultrasonic dispersion for 5min at the beginning stage of sanding;
2) pre-burning: pre-sintering the powder in the last step at 900 ℃, immediately transferring to an environment of 25 ℃ after heat preservation, and rapidly cooling to room temperature;
3) sanding: adding the auxiliary components into the pre-sintered material treated in the previous step, then performing sand milling and mixing, controlling the particle size to be 1.0 mu m, and performing auxiliary ultrasonic dispersion for 10min at the beginning stage of sand milling;
4) granulating and forming;
5) and (3) sintering: and sintering the formed blank in an equilibrium oxygen partial pressure at the sintering temperature of 1200 ℃ and the cooling rate of 3.5 ℃/min in a cooling stage below 1100 ℃.
Example 2: a high-frequency low-loss Mn-Zn ferrite material for fine tuning ferrous ions is composed of main component and auxiliary component, the main component is Fe2O358mol%, ZnO 4mol%, MgO 0.2mol%, MnO 37.8mol%, all examples and comparative examples are the same minor components.
The preparation method comprises the following steps:
1) preparing materials: according to the quaternary system formula, weighing Fe in a corresponding proportion2O3ZnO, MgO and MnO, then sanding for 15min, and performing auxiliary ultrasonic dispersion for 5min at the beginning stage of sanding;
2) pre-burning: pre-sintering the powder in the last step at 900 ℃, immediately transferring to an environment of 25 ℃ after heat preservation, and rapidly cooling to room temperature;
3) sanding: adding the auxiliary components into the pre-sintered material treated in the previous step, then performing sand milling and mixing, controlling the particle size to be 1.0 mu m, and performing auxiliary ultrasonic dispersion for 10min at the beginning stage of sand milling;
4) granulating and forming;
5) and (3) sintering: and sintering the formed blank in an equilibrium oxygen partial pressure at the sintering temperature of 1200 ℃ and the cooling rate of 3.5 ℃/min in a cooling stage below 1100 ℃.
Example 3: a high-frequency low-loss Mn-Zn ferrite material for fine tuning ferrous ions is composed of main component and auxiliary component, the main component is Fe2O360mol%, ZnO 1mol%, MgO 0.3mol%, MnO 38.7mol%, all examples and comparative examples are the same subcomponents.
The preparation method comprises the following steps:
1) preparing materials: according to the quaternary system formula, weighing Fe in a corresponding proportion2O3ZnO, MgO and MnO, then sanding for 15min, and performing auxiliary ultrasonic dispersion for 5min at the beginning stage of sanding;
2) pre-burning: pre-sintering the powder in the last step at 900 ℃, immediately transferring to an environment of 25 ℃ after heat preservation, and rapidly cooling to room temperature;
3) sanding: adding the auxiliary components into the pre-sintered material treated in the previous step, then performing sand milling and mixing, controlling the particle size to be 1.0 mu m, and performing auxiliary ultrasonic dispersion for 10min at the beginning stage of sand milling;
4) granulating and forming;
5) and (3) sintering: and sintering the formed blank in an equilibrium oxygen partial pressure at the sintering temperature of 1200 ℃ and the cooling rate of 4 ℃/min in a cooling stage below 1100 ℃.
Comparative example 1: a high-frequency low-loss Mn-Zn ferrite material without fine-tuning ferrous ions is composed of main component and auxiliary component, the main component is Fe2O356.1mol%, ZnO 4mol%, MnO 39.9mol%, and all examples and comparative examples are the same subcomponents.
The preparation method comprises the following steps:
1) preparing materials: according to the quaternary system formula, weighing Fe in a corresponding proportion2O3ZnO, MgO and MnO, followed by sanding15min, and carrying out auxiliary ultrasonic dispersion for 5min at the beginning stage of sanding;
2) pre-burning: pre-sintering the powder in the last step at 900 ℃, immediately transferring to an environment of 25 ℃ after heat preservation, and rapidly cooling to room temperature;
3) sanding: adding the auxiliary components into the pre-sintered material treated in the previous step, then performing sand milling and mixing, controlling the particle size to be 1.0 mu m, and performing auxiliary ultrasonic dispersion for 10min at the beginning stage of sand milling;
4) granulating and forming;
5) and (3) sintering: and sintering the formed blank in an equilibrium oxygen partial pressure at the sintering temperature of 1200 ℃ and the cooling rate of 3.5 ℃/min in a cooling stage below 1100 ℃.
Comparative example 2: a high-frequency low-loss Mn-Zn ferrite material without fine-tuning ferrous ions is composed of main component and auxiliary component, the main component is Fe2O360.3mol%, ZnO 1mol%, MnO 38.7 mol%; the subcomponents were conventional dopants in the ferrite field, and all the examples and comparative examples were the same subcomponents.
The preparation method comprises the following steps:
1) preparing materials: according to the quaternary system formula, weighing Fe in a corresponding proportion2O3ZnO, MgO and MnO, then sanding for 15min, and performing auxiliary ultrasonic dispersion for 5min at the beginning stage of sanding;
2) pre-burning: pre-sintering the powder in the last step at 900 ℃, immediately transferring to an environment of 25 ℃ after heat preservation, and rapidly cooling to room temperature;
3) sanding: adding the auxiliary components into the pre-sintered material treated in the previous step, then performing sand milling and mixing, controlling the particle size to be 1.0 mu m, and performing auxiliary ultrasonic dispersion for 10min at the beginning stage of sand milling;
4) granulating and forming;
5) and (3) sintering: and sintering the formed blank in an equilibrium oxygen partial pressure at the sintering temperature of 1200 ℃ and the cooling rate of 4 ℃/min in a cooling stage below 1100 ℃.
Comparative example 3: a high-frequency low-loss Mn-Zn ferrite material for fine tuning ferrous ions is composed of main component and auxiliary component, the main component is Fe2O356mol percent, 4mol percent of ZnO, 0.1mol percent of MgO and 39.9mol percent of MnO; the subcomponents were conventional dopants in the ferrite field, and all the examples and comparative examples were the same subcomponents.
The preparation method comprises the following steps:
1) preparing materials: according to the quaternary system formula, weighing Fe in a corresponding proportion2O3ZnO, MgO and MnO, and then sanding for 15min without assisting other dispersion modes;
2) pre-burning: pre-sintering the powder in the last step at 900 ℃, immediately transferring to an environment of 25 ℃ after heat preservation, and rapidly cooling to room temperature;
3) sanding: adding the auxiliary components into the pre-sintered material treated in the previous step, and then performing sand milling and mixing, wherein the particle size is controlled to be 1.0 mu m, and other dispersion modes are not assisted;
4) granulating and forming;
5) and (3) sintering: and sintering the formed blank in an equilibrium oxygen partial pressure at the sintering temperature of 1200 ℃ and the cooling rate of 3.5 ℃/min in a cooling stage below 1100 ℃.
Comparative example 4: a high-frequency low-loss Mn-Zn ferrite material for fine tuning ferrous ions is composed of main component and auxiliary component, the main component is Fe2O356mol percent, 4mol percent of ZnO, 0.1mol percent of MgO and 39.9mol percent of MnO; the subcomponents were conventional dopants in the ferrite field, and all the examples and comparative examples were the same subcomponents.
The preparation method comprises the following steps:
1) preparing materials: according to the quaternary system formula, weighing Fe in a corresponding proportion2O3ZnO, MgO and MnO, then sanding for 15min, and performing auxiliary ultrasonic dispersion for 5min at the beginning stage of sanding;
2) pre-burning: pre-burning the powder in the last step at 900 deg.c, and cooling in the furnace;
3) sanding: adding the auxiliary components into the pre-sintered material treated in the previous step, then performing sand milling and mixing, controlling the particle size to be 1.0 mu m, and performing auxiliary ultrasonic dispersion for 10min at the beginning stage of sand milling;
4) granulating and forming;
5) and (3) sintering: and sintering the formed blank in an equilibrium oxygen partial pressure at the sintering temperature of 1200 ℃ and the cooling rate of 1.5 ℃/min in a cooling stage below 1100 ℃.
The results of the ring performance test of the standard samples prepared in the above examples and comparative examples are as follows:
Figure 665447DEST_PATH_IMAGE002
comparative example 1 no fine tuning of ferrous ions compared to example 1, the power consumption was higher, especially 100 ℃.
Comparative example 2 did not fine tune ferrous ions compared to example 3 and the power consumption was higher, especially 100 ℃.
Comparative example 3 fine-tuned the ferrous ions compared to example 1, but the mixing process did not assist ultrasonic dispersion and the power consumption increased.
Comparative example 4 fine-tuned the ferrous ions compared to example 1, but the pre-firing and cool-down stages did not cool down rapidly and the power consumption increased somewhat.

Claims (8)

1. The high-frequency low-loss manganese-zinc ferrite material for fine adjustment of ferrous ions is characterized in that: the main component of the material is a quaternary system, and simultaneously, an iron-rich formula is adopted, namely Fe2O3Y-X mol% (55 is less than or equal to 60), ZnO is less than 5 mol%, MgO is X mol% (X is less than or equal to 0.4), and the balance is MnO, and the preparation method can avoid magnesium element precipitation, and the material preparation method comprises the following steps:
(1) preparing materials: fe was weighed according to the quaternary formula2O3And ZnO, MgO and MnO, and then carrying out sand grinding and mixing, and simultaneously carrying out ultrasonic dispersion treatment;
(2) pre-burning: pre-burning the powder in the last step at 800-1000 ℃, immediately transferring to an environment of 25 ℃ after heat preservation, and rapidly cooling to room temperature;
(3) sanding: adding the auxiliary components into the pre-sintered material treated in the previous step, and then performing sand grinding and mixing while assisting with ultrasonic dispersion treatment;
(4) granulating and forming;
(5) and (3) sintering: and (3) sintering the formed blank in an equilibrium oxygen partial pressure at the sintering temperature of 1100-1300 ℃ for 3-5 h, wherein the cooling rate of a cooling stage below 1100 ℃ is 2-6 ℃/min.
2. The high-frequency low-loss manganese-zinc ferrite material for finely adjusting ferrous ions according to claim 1, characterized in that a trace amount of Mg ions can be used to replace Fe ions to achieve the purpose of finely adjusting ferrous ions, Y is more than or equal to 55 and less than or equal to 57, and X is more than or equal to 0.1 and less than or equal to 0.3.
3. The ferrous ion fine-tuning high-frequency low-loss manganese-zinc ferrite material according to claim 1, wherein in the step (1), the sanding time is 10-20 min.
4. The ferrous ion fine-tuning high-frequency low-loss manganese-zinc ferrite material according to claim 1, wherein in the step (1) and the step (3), the ultrasonic dispersion is carried out for 3min-15 min.
5. The ferrous ion fine-tuning high-frequency low-loss manganese-zinc ferrite material according to claim 1, wherein in the step (2), the pre-sintering temperature is 850-950 ℃, and the temperature is kept for 1-3 h.
6. The ferrous ion fine-tuning high-frequency low-loss manganese-zinc ferrite material according to claim 1, wherein in the step (3), the particle size of the material after sanding is 0.8-1.8 μm.
7. The ferrous ion fine-tuning high-frequency low-loss manganese-zinc ferrite material as claimed in claim 1, wherein in the step (5), the cooling rate in the cooling stage below 1100 ℃ is between 3 ℃/min and 5 ℃/min.
8. The ferrous ion fine-tuning high frequency low loss manganese-zinc ferrite material of any one of claims 1 to 7, wherein said subcomponent may be Co2O3、TiO2、CaCO3、ZrO2、V2O5、Ta2O5、Nb2O5、CuO、SnO2In the following content ranges: co2O3：0-0.8wt%、TiO2：0-1wt%、CaCO3：0.01-0.2wt%、ZrO2：0-0.02wt%、V2O5：0.01-0.05wt%、Ta2O5：0.01-0.05wt%、Nb2O5：0.01-0.03wt%、CuO：0-0.02wt%、SnO2：0-0.02wt%。
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