CN115536379B - High-frequency low-loss soft magnetic ferrite material and preparation method and application thereof - Google Patents

High-frequency low-loss soft magnetic ferrite material and preparation method and application thereof Download PDF

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CN115536379B
CN115536379B CN202211303561.XA CN202211303561A CN115536379B CN 115536379 B CN115536379 B CN 115536379B CN 202211303561 A CN202211303561 A CN 202211303561A CN 115536379 B CN115536379 B CN 115536379B
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soft magnetic
magnetic ferrite
frequency low
ferrite material
temperature
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CN115536379A (en
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王育伟
张维
高庞
王荣杰
卜简
张祥
赵富平
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Suzhou Tianyuan Magnetic Materials Co ltd
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Abstract

The invention belongs to the technical field of soft magnetic ferrite, and particularly relates to a high-frequency low-loss soft magnetic ferrite material, and a preparation method and application thereof. The invention provides a high-frequency low-loss soft magnetic ferrite material, which comprises a main component and an auxiliary component; the main component is 58 to 62mol percent of Fe 2 O 3 And 38-42mol% MnO. The ZnO component is removed from the high-frequency low-loss soft magnetic ferrite material provided by the invention, and only Fe is used 2 O 3 And MnO as a main component, and controls Fe 2 O 3 The MnO proportion is in a proper range, and the high-frequency low-power loss performance of the material can still be realized. And the preparation process of the traditional MnZn ferrite is not required to be changed.

Description

High-frequency low-loss soft magnetic ferrite material and preparation method and application thereof
Technical Field
The invention belongs to the technical field of soft magnetic ferrite, and particularly relates to a high-frequency low-loss soft magnetic ferrite material, and a preparation method and application thereof.
Background
Soft magnetic ferrite materials and cores prepared therefrom are widely used in the technical field of high frequency power electronics due to their high resistivity, high frequency and low power loss. The low-power loss magnetic core can reduce the temperature rise of the electronic device and improve the energy conversion efficiency of the electronic device. Meanwhile, in order to reduce the size of electronic devices, the operating frequency of ferrite cores is also increasing, and some cores have an operating frequency exceeding 1MHz. To date, intensive studies have been conducted on the formulation design, preparation process optimization, structural design, and the like of conventional MnZn ferrite materials in order to obtain a soft magnetic ferrite core with high frequency and low power loss.
For example, the prior art discloses a high saturation magnetic flux density soft magnetic ferrite material, which comprises a main material component and an auxiliary material component, wherein the main material component comprises 59.5-61.5mol% of ferric oxide, 23.5-27.5mol% of manganese oxide, 10.5-11.5mol% of zinc oxide and the balance of lithium carbonate according to mole percentage.
The main component of the existing MnZn ferrite is composed of Fe2O3, mnO and ZnO in terms of oxide, but ZnO is a non-magnetic component, and excessive addition of the ZnO can reduce the magnetic property of the material on one hand, and on the other hand, the ZnO has higher price, so that the cost of the product is not reduced.
Disclosure of Invention
Therefore, the invention aims to overcome the defects that the soft magnetic ferrite material in the prior art contains ZnO as a non-magnetic component, and excessive addition of the ZnO reduces the magnetic performance of the material on one hand and the price of the ZnO is higher on the other hand, which is unfavorable for the reduction of the product cost, thereby providing a high-frequency low-loss soft magnetic ferrite material and a preparation method and application thereof.
Therefore, the invention provides the following technical proposal,
the invention provides a high-frequency low-loss soft magnetic ferrite material, which comprises a main component and an auxiliary component;
the main component is 58 to 62mol percent of Fe 2 O 3 And 38-42mol% MnO.
In the soft magnetic ferrite material, as a preferred embodiment, the subcomponents are CaO in an amount of 500 to 1500ppm and Sb in an amount of 100 to 1500ppm based on the mass percentage of the main component 2 O 3 50-500ppm ZrO 2 And 50-500ppm Nb 2 O 5 。
The invention also provides a preparation method of the high-frequency low-loss soft magnetic ferrite material, which comprises the following steps:
s1: mixing the main component raw materials, presintering, adding the auxiliary component raw materials, grinding, adding a binder, and granulating to obtain a formed body;
s2: after sintering the obtained molded body, cooling to room temperature in the atmosphere of protective gas to obtain the high-frequency low-loss soft magnetic ferrite material;
wherein, in the sintering process, the oxygen partial pressure concentration between the temperature rise from 900 ℃ and the sintering temperature is controlled to be below 3.0%.
Specifically, the sintering process comprises the following stages:
the first stage, when the temperature is raised to 900 ℃ from room temperature, the temperature raising rate is 0.5-2 ℃/min, and the temperature raising process in the first stage is carried out under the atmosphere;
a second stage, wherein when the temperature is increased from 900 ℃ to the sintering temperature, the temperature increasing rate is 0.5-1 ℃/min, and the oxygen partial pressure concentration in the second stage is 0-3.0%;
and in the third stage, the oxygen partial pressure concentration in the stage is 1.5-21% when the sintering is carried out at the sintering temperature.
In the above preparation method, as a preferred embodiment, the sintering temperature is 1050-1150 ℃;
and/or the sintering time is 0.5-8h.
In the above preparation method, as a preferred embodiment, the mixing is wet mixing, and the mixing medium of the wet mixing is water;
the wet mixing time is 0.5-2 h.
In the above preparation method, as a preferred embodiment, the pre-firing time is 0.5 to 5 hours;
and/or, the presintering temperature is 700-950 ℃.
In the above preparation method, as a preferred embodiment, the grinding adopts wet grinding, and the grinding medium of the wet grinding is water;
the wet grinding time is 0.5-5h.
In the above preparation method, as a preferred embodiment, the binder includes at least one of polyvinyl alcohol, carboxymethyl cellulose, polyvinyl acetate;
the granulation adopts spray granulation;
the protective gas comprises one of nitrogen and argon.
The invention also provides an application of the high-frequency low-loss soft magnetic ferrite material or the high-frequency low-loss soft magnetic ferrite material obtained by the preparation method in the annular magnetic core.
In the above application, as a preferred embodiment, the toroidal core is prepared such that a standard core having a power loss of 300kW/m at 100℃at 1MHz/50mT is prepared such that a.di. 25.times.15.times.7 3 The following is given.
The technical scheme provided by the invention has the following advantages:
1. the invention provides a high-frequency low-loss soft magnetic ferrite material, which comprises a main component and an auxiliary component; the main component is 58 to 62mol percent of Fe 2 O 3 And 38-42mol% MnO. The ZnO component is removed from the high-frequency low-loss soft magnetic ferrite material provided by the invention, and only Fe is used 2 O 3 And MnO as a main component, and controls Fe 2 O 3 The MnO proportion is in a proper range, and the high-frequency low-power loss performance of the material can still be realized. And the preparation process of the traditional MnZn ferrite is not required to be changed.
2. The present invention strictly controls the content of the subcomponents because the applicant found that the above subcomponents are present in grain boundaries, and the grain boundary resistivity is improved, and the eddy current loss is reduced, thereby reducing the total loss. When the content of the above auxiliary components is lower than the lower limit value, the grain boundary resistivity cannot be effectively improved, and the effect of reducing loss cannot be achieved; when the content of the above subcomponents exceeds the upper limit value, abnormal growth of crystal grains tends to occur, and loss is deteriorated.
3. The invention further controls the loss performance of the material by controlling the temperature and the oxygen partial pressure in the sintering process. When the temperature is lower than 900 ℃, the partial pressure of oxygen is lower, which is not beneficial to the discharge of the molding adhesive, and on the other hand, the production cost is increased due to the fact that inert protective gas is required to be flushed in too early; when the temperature is above 900 ℃, the low oxygen partial pressure is controlled, which is unfavorable for the completion of the solid phase reaction of the sintered body, the densification degree is low, and the loss is deteriorated.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Example 1
The embodiment provides a preparation method of a high-frequency low-loss soft magnetic ferrite material, which comprises the following steps:
will consist of 59 mol% Fe 2 O 3 Raw materials composed of 41 mol% MnO were mixed in a sand mill for 1 hour, and then pre-burned at 850 ℃ for 2 hours. Based on the mass of the powder after presintering, adding auxiliary components into the presintering material, wherein the added auxiliary components are as follows: 1000ppm CaO,500ppm Sb 2 O 3 300ppm ZrO 2 And 300ppm Nb 2 O 5 . Then carrying out secondary sanding for 2 hours, adding polyvinyl alcohol, then carrying out spray granulation, and then carrying out sintering, wherein in the sintering process, the temperature is firstly increased to 900 ℃ from room temperature at a heating rate of 2 ℃/min, and the temperature is increased in the atmosphere; then the temperature is increased from 900 ℃ to 1100 ℃ with the temperature increasing rate of 1.0 ℃/min, and the oxygen partial pressure in the temperature increasing stage is maintained at 0.5%; maintaining the temperature at 1100 ℃ for 5 hours and maintaining the oxygen partial pressure at 1.5%; and finally, cooling to room temperature under the condition of maintaining the equilibrium oxygen partial pressure under the condition of deluxe of nitrogen, and obtaining the high-frequency low-loss soft magnetic ferrite material.
The high-frequency low-loss soft magnetic ferrite material prepared in example 1 was made into a standard magnetic core of.25.times.15.times.7, and then the power loss of the standard magnetic core was tested at 1MHz/50mT and 100℃by using a SY8219 type B-H analyzer, resulting in 204kW/m 3 。
Example 2
The embodiment provides a preparation method of a high-frequency low-loss soft magnetic ferrite material, which comprises the following steps:
will consist of 60mol% Fe 2 O 3 Raw materials composed of 40 mol% MnO were mixed in a sand mill for 1 hour, and then pre-burned at 850 ℃ for 2 hours. Based on the mass of the powder after presintering, adding auxiliary components into the presintering material, wherein the added auxiliary components are as follows: 800ppm CaO,600ppm Sb 2 O 3 ZrO of 200ppm 2 And 200ppm Nb 2 O 5 . Then carrying out secondary sanding for 2 hours, adding polyvinyl alcohol, then carrying out spray granulation, and then carrying out sintering, wherein in the sintering process, the temperature is firstly increased to 900 ℃ from room temperature at a heating rate of 2 ℃/min, and the temperature is increased in the atmosphere; then, the temperature is increased from 900 ℃ to 1130 ℃ with the temperature increasing rate of 1.0 ℃/min, and the oxygen partial pressure in the temperature increasing stage is maintained at 0.5%; maintaining the temperature at 1130 ℃ for 5 hours and maintaining the oxygen partial pressure at 1.5%; and finally, cooling to room temperature under the condition of maintaining the equilibrium oxygen partial pressure under the condition of deluxe of nitrogen, and obtaining the high-frequency low-loss soft magnetic ferrite material.
The high-frequency low-loss soft magnetic ferrite material prepared in example 2 was made into a standard magnetic core of.25.times.15.times.7, and then the power loss of the standard magnetic core was tested at 1MHz/50mT and 100℃by using a SY8219 type B-H analyzer, resulting in 192kW/m 3 。
Example 3
The embodiment provides a preparation method of a high-frequency low-loss soft magnetic ferrite material, which comprises the following steps:
will consist of 61mol% Fe 2 O 3 Raw materials composed of 39 mol% MnO were mixed in a sand mill for 1 hour, and then pre-burned at 850 ℃ for 2 hours. Based on the mass of the powder after presintering, adding auxiliary components into the presintering material, wherein the added auxiliary components are as follows: 900ppm CaO,400ppm Sb 2 O 3 250ppm ZrO 2 And 250ppm Nb 2 O 5 . Then carrying out secondary sanding for 2 hours, adding polyvinyl alcohol, then carrying out spray granulation, and then carrying out sintering, wherein in the sintering process, the temperature is firstly increased to 900 ℃ from room temperature at a heating rate of 2 ℃/min, and the temperature is firstly increasedIn an atmosphere; then the temperature is increased from 900 ℃ to 1060 ℃, the heating rate is 1.0 ℃/min, and the oxygen partial pressure in the heating stage is maintained at 0.5%; maintaining the temperature at 1060 ℃ for 5 hours and maintaining the oxygen partial pressure at 1.5%; and finally, cooling to room temperature under the condition of maintaining the equilibrium oxygen partial pressure under the condition of deluxe of nitrogen, and obtaining the high-frequency low-loss soft magnetic ferrite material.
The high-frequency low-loss soft magnetic ferrite material prepared in example 3 was made into a standard core of.25.times.15.times.7, and then the power loss of the standard core was tested at 1MHz/50mT and 100℃using a SY8219 type B-H analyzer, resulting in 187kW/m 3 。
Example 4
The embodiment provides a preparation method of a high-frequency low-loss soft magnetic ferrite material, which comprises the following steps:
the difference between this example and example 2 is that the subcomponent CaO is 2000ppm.
The high-frequency low-loss soft magnetic ferrite material prepared in example 4 was made into a standard magnetic core of.25×15×7, and then the power loss of the standard magnetic core was tested at 1MHz/50mT and 100℃using a SY8219 type B-H analyzer, resulting in 732kW/m 3 。
Example 5
The embodiment provides a preparation method of a high-frequency low-loss soft magnetic ferrite material, which comprises the following steps:
the difference between this example and example 2 is that the subcomponent Sb 2 O 3 2000ppm.
The high-frequency low-loss soft magnetic ferrite material prepared in example 5 was made into a standard magnetic core of.25.times.15.times.7, and then the power loss of the standard magnetic core was tested at 1MHz/50mT and 100℃by using a SY8219 type B-H analyzer, resulting in 574kW/m 3 。
Example 6
The embodiment provides a preparation method of a high-frequency low-loss soft magnetic ferrite material, which comprises the following steps:
this example is different from example 3 in that the temperature is increased from 900 to 1060 ℃ again, the heating rate is 1.0 ℃/min, and the oxygen partial pressure in the heating stage is maintained at 4.0%.
The high-frequency low-loss soft magnetic ferrite material prepared in example 6 was made into a standard magnetic core of.25×15×7, and then the power loss of the standard magnetic core was tested at 1MHz/50mT and 100℃using a SY8219 type B-H analyzer, resulting in 536kW/m 3 。
Example 7
The embodiment provides a preparation method of a high-frequency low-loss soft magnetic ferrite material, which comprises the following steps:
this example differs from example 3 in that the partial pressure of oxygen is maintained at 5.0% when incubated at 1060℃for 5 hours.
The high-frequency low-loss soft magnetic ferrite material prepared in example 7 was made into a standard magnetic core of.25×15×7, and then the power loss of the standard magnetic core was tested at 1MHz/50mT and 100℃using a SY8219 type B-H analyzer, resulting in 491kW/m 3 。
Comparative example 1
The comparative example provides a preparation method of a high-frequency low-loss soft magnetic ferrite material, which comprises the following steps:
the comparative example is different from example 1 in that the main component is 56mol% Fe 2 O 3 And 44 mol% MnO.
The high-frequency low-loss soft magnetic ferrite material prepared in comparative example 1 was made into a standard magnetic core of.25.times.15.times.7, and then the power loss of the standard magnetic core was tested at 1MHz/50mT and 100℃by using a SY8219 type B-H analyzer, resulting in 418kW/m 3 。
Comparative example 2
The comparative example provides a preparation method of a high-frequency low-loss soft magnetic ferrite material, which comprises the following steps:
the comparative example is different from example 1 in that the main component is 65mol% Fe 2 O 3 And 35mol% MnO.
The high-frequency low-loss soft magnetic ferrite material prepared in comparative example 2 was made into a standard magnetic core of.25.times.15.times.7, and then the power loss of the standard magnetic core was tested at 1MHz/50mT and 100℃by using a SY8219 type B-H analyzer, resulting in 632kW/m 3 。
The above embodiments are only for illustrating the technical concept and features of the present invention, and are intended to enable those skilled in the art to understand the present invention and to implement the same, but are not intended to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be included in the scope of the present invention.

Claims (9)

1. A high-frequency low-loss soft magnetic ferrite material is obtained by sintering a molded body,
the high-frequency low-loss soft magnetic ferrite material is characterized by comprising a main component and an auxiliary component;
the main component is 58 to 62mol percent of Fe 2 O 3 And 38-42mol% MnO;
the auxiliary components comprise 500-1500ppm of CaO and 100-1500ppm of Sb by mass percent of the main components 2 O 3 50-500ppm ZrO 2 And 50-500ppm Nb 2 O 5 ；
The sintering process comprises the following stages:
the first stage, when the temperature is raised to 900 ℃ from room temperature, the temperature raising rate is 0.5-2 ℃/min, and the temperature raising process in the first stage is carried out under the atmosphere;
a second stage, wherein when the temperature is increased from 900 ℃ to the sintering temperature, the temperature increasing rate is 0.5-1 ℃/min, and the oxygen partial pressure concentration in the second stage is 0-3.0%;
and in the third stage, the oxygen partial pressure concentration in the stage is 1.5-21% when the sintering is carried out at the sintering temperature.
2. A method of preparing the high frequency low loss soft magnetic ferrite material of claim 1, comprising the steps of:
s1: mixing the main component raw materials, presintering, adding the auxiliary component raw materials, grinding, adding a binder, and granulating to obtain a formed body;
s2: after sintering the obtained molded body, cooling to room temperature in the atmosphere of protective gas to obtain the high-frequency low-loss soft magnetic ferrite material;
wherein, in the sintering process, the oxygen partial pressure concentration between the temperature rise from 900 ℃ and the sintering temperature is controlled to be below 3.0%.
3. The method for preparing a high-frequency low-loss soft magnetic ferrite material according to claim 2, wherein the sintering temperature is 1050-1150 ℃;
and/or the sintering time is 0.5-8h.
4. The method for producing a high-frequency low-loss soft magnetic ferrite material according to claim 2, wherein the mixing is performed by wet mixing, and the mixing medium of the wet mixing is water;
the wet mixing time is 0.5-2 h.
5. The method for preparing a high-frequency low-loss soft magnetic ferrite material according to claim 2, wherein the presintering time is 0.5-5h;
and/or, the presintering temperature is 700-950 ℃.
6. The method for producing a high-frequency low-loss soft magnetic ferrite material according to claim 2, wherein the grinding is wet grinding, and the grinding medium of the wet grinding is water;
the wet grinding time is 0.5-5h.
7. The method for producing a high-frequency low-loss soft magnetic ferrite material according to claim 2, wherein the binder comprises at least one of polyvinyl alcohol, carboxymethyl cellulose, polyvinyl acetate;
the granulation adopts spray granulation;
the protective gas comprises one of nitrogen and argon.
8. Use of a high frequency low loss soft magnetic ferrite material according to claim 1 or obtained by the method of any one of claims 2 to 7 in a toroidal core.
9. The use according to claim 8, characterized in that the toroidal core is prepared as a standard core of Φ25X15X107 with a power loss of 300kW/m at 1MHz/50mT at 100 DEG C 3 The following is given.
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