A manganese-zinc power ferrite material, a preparation method and application thereof

Abstract

The present application relates to a kind of manganese zinc power ferrite material and its preparation method and application, the manganese zinc power ferrite material includes main component and additive, the main component includes Fe2O3, ZnO and MnO, the additive is composed of SnO2, CaCO3, ZrO2 And Co2O3.The present application is by the cooperation between each additive and the content control, and the raw material ratio of main component is combined, and then the component of manganese zinc power ferrite material is controlled, and combined with additive step-by-step mixing sintering process, so that the manganese zinc power ferrite material in 25~160 ℃ ultra-wide temperature range overall loss is low, i.e., in 100kHz, 200mT condition 25 ℃ power consumption≤360kW / m 3 , 100 ℃ power consumption≤310kW / m 3 , 160 ℃ power consumption≤360kW / m 3 .

Description

Technical Field

[0001] This invention relates to the field of ferrite materials technology, and in particular to a manganese-zinc power ferrite material, its preparation method, and its application. Background Technology

[0002] In recent years, with the increasing awareness of environmental protection, the electric vehicle industry has also ushered in a good development opportunity. The DC-DC converters used in electric vehicles (EVs), hybrid electric vehicles (HEVs), and fuel cell electric vehicles (FCEVs) urgently need a manganese-zinc ferrite material with low loss over an ultra-wide temperature range due to the special nature of their operation. This is mainly because the speed of a car is constantly changing during driving, which causes the load output power to change constantly. In addition, due to differences in regional environment and season, the ambient temperature range of the car's operation is also very large, so the temperature of the switching power supply will change constantly over a wide temperature range.

[0003] CN102693807A discloses an ultra-wide temperature range, low loss, high flux density MnZn power ferrite and its preparation method. The main components of the ferrite magnetic material include: Fe2O3: 52-53 mol%, ZnO: 10-12 mol%, MnO: 36-37 mol%. Additives include: CaCO3: 0.01-0.07 wt%, SnO2: 0.01-0.2 wt%, Nb2O5: 0.01-0.04 wt%, ZrO2: 0.01-0.04 wt%, Co2O3: 0.2-0.55 wt%, and V2O5: 0.01-0.05 wt%. The loss Pcv under 100 kHz and 200 mT conditions is: power consumption < 390 kW / m at 25℃. 3 Power consumption at 120℃ < 330kW / m 3 Power consumption at 140℃ < 400kW / m 3 It only disclosed the power consumption below 140℃, and did not involve the power consumption above 140℃, and its high-temperature loss was significantly higher.

[0004] CN102693803A discloses a wide-temperature, low-loss MnZn power ferrite and its preparation method. The composition, calculated by oxides, is: Fe2O3: 51–54 mol%, MnO: 35–38 mol%, ZnO: 9–13 mol%. The auxiliary components, based on the total weight of the main components, are: CaCO3: 0.03–0.1 wt%, SnO2: 0.02–0.1 wt%, Nb2O5: 0.01–0.04 wt%, ZrO2: 0.01–0.05 wt%, and Co2O3: 0.1–0.5 wt%. Under conditions of 100 kHz and 200 mT at 25℃–120℃, the power consumption at 25℃ is ≤350 mW / cm². 3Power consumption at 120℃ ≤350mW / cm 3 It only disclosed the power consumption below 120℃, and did not involve the power consumption above 120℃, and its high-temperature loss is still significantly high.

[0005] Therefore, how to provide a manganese-zinc ferrite material with low overall loss over an ultra-wide temperature range of 25–160℃, especially with low loss under high temperature conditions of 160℃, has become an urgent problem to be solved. It is of great significance to meet the needs of switching power supplies under complex conditions. Summary of the Invention

[0006] To address the aforementioned technical problems, this invention provides a manganese-zinc power ferrite material, its preparation method, and its applications. This invention regulates the composition of the manganese-zinc power ferrite material by controlling the combination and content of various additives, and by adjusting the raw material ratio of the main components. Furthermore, by employing a stepwise mixing and sintering process for the additives, the overall power loss of the manganese-zinc power ferrite material is kept low over an ultra-wide temperature range of 25–160°C. Specifically, at 100 kHz and 200 mT, the power consumption at 25°C is ≤360 kW / m. 3 Power consumption at 100℃ ≤ 310kW / m 3 Power consumption at 160℃ ≤360kW / m 3 .

[0007] To achieve this objective, the present invention adopts the following technical solution:

[0008] In a first aspect, the present invention provides a manganese-zinc power ferrite material, the manganese-zinc power ferrite material comprising a main component and additives, the main component comprising Fe2O3, ZnO and MnO, and the additives comprising SnO2, CaCO3, ZrO2 and Co2O3.

[0009] In this invention, the combined addition of four additives—SnO2, CaCO3, ZrO2, and Co2O3—enables the manganese-zinc power ferrite material to exhibit wide temperature range and low loss characteristics, especially at a high temperature of 160°C, where it still maintains low loss.

[0010] The combined addition of CaCO3 and ZrO2 acts at the grain boundaries, forming a high-resistivity layer to increase grain boundary resistivity, thereby reducing eddy current losses and improving high-temperature losses. Furthermore, the addition of CaCO3 and ZrO2 can also improve grain uniformity and reduce porosity, thus lowering both eddy current and hysteresis losses. The combined addition of SnO2 and Co2O3 acts within the grains, with Sn… 4+ With a portion of Fe 2+ Formation of Sn 4+ -Fe 2+Ion pairs, inhibiting Fe 2+ with Fe 3+ Electron transitions between Co2O3 and Fe increase the resistivity within the grain and reduce eddy current losses; while Co2O3 and Fe 2+ The synergistic effect is achieved because Co2O3 has a positive K1 (magnetic anisotropy constant), which compensates for the negative K1 value of the manganese-zinc power ferrite material, causing the magnetocrystalline anisotropy constant to tend to 0, thereby reducing hysteresis loss.

[0011] This invention achieves low overall loss within a wide temperature range of 25–160°C by combining the above-mentioned additives, which work simultaneously at grain boundaries and within grains. Combined with the raw material ratio of the main components, this invention maintains low loss even at high temperatures of 160°C.

[0012] As a preferred technical solution of the present invention, the Fe2O3 content is 69.50-69.68 wt%, based on the mass of the main component as 100%, for example, 69.50 wt%, 69.52 wt%, 69.55 wt%, 69.58 wt%, 69.60 wt%, 69.62 wt%, 69.65 wt%, or 69.68 wt%, etc.

[0013] Preferably, the ZnO content is 5.5 to 6.4 wt%, for example, 5.5 wt%, 5.8 wt%, 6 wt%, 6.2 wt%, or 6.4 wt%, based on the mass of the main component as 100%.

[0014] Preferably, the mass of MnO is 23.6 to 25.4 wt%, based on the mass of the main component as 100%, for example, 23.6 wt%, 23.7 wt%, 23.8 wt%, 23.9 wt%, 24.0 wt%, 24.1 wt%, 24.2 wt%, 24.3 wt%, 24.4 wt%, 24.5 wt%, 24.6 wt%, 24.7 wt%, 24.8 wt%, 24.9 wt%, 25.0 wt%, 25.1 wt%, 25.2 wt%, 25.3 wt%, or 25.4 wt%, etc.

[0015] In this invention, based on the combination of SnO2, CaCO3, ZrO2, and Co2O3 additives, the overall loss of the manganese-zinc power ferrite material is kept low over an ultra-wide temperature range of 25–160℃ by adjusting the content of the main components. Specifically, at 100kHz and 200mT, the power consumption at 25℃ is ≤360kW / m. 3 Power consumption at 100℃ ≤ 310kW / m 3 Power consumption at 160℃ ≤360kW / m 3 .

[0016] Preferably, based on the total mass of the main components, the amount of SnO2 added is 1000 to 2000 ppm, such as 1000 ppm, 1200 ppm, 1400 ppm, 1600 ppm, 1800 ppm or 2000 ppm.

[0017] Preferably, the amount of CaCO3 added is 500 to 1200 ppm, based on the total mass of the main components, for example, 500 ppm, 600 ppm, 700 ppm, 800 ppm, 900 ppm, 1000 ppm, 1100 ppm or 1200 ppm.

[0018] Preferably, the amount of ZrO2 added is 100 to 400 ppm, based on the total mass of the main component, for example, 100 ppm, 150 ppm, 200 ppm, 250 ppm, 300 ppm, 350 ppm or 400 ppm.

[0019] Preferably, the amount of Co2O3 added is 3000 to 4500 ppm, based on the total mass of the main components, for example, 3000 ppm, 3300 ppm, 3500 ppm, 3800 ppm, 4000 ppm, 4200 ppm or 4500 ppm.

[0020] As a preferred embodiment of the present invention, the manganese-zinc power ferrite material has a power consumption of ≤360kW / m at 25℃ under conditions of 100kHz and 200mT within a temperature range of 25~160℃. 3 Power consumption at 100℃ ≤ 310kW / m 3 Power consumption at 160℃ ≤360kW / m 3 .

[0021] In a second aspect, the present invention also provides a method for preparing the manganese-zinc power ferrite material according to the first aspect, the method comprising the following steps:

[0022] (1) Mix the main component and the first additive evenly, and then pre-calcine to obtain the pre-calcined material;

[0023] (2) The pre-burned material described in step (1) is mixed evenly with the second additive to obtain intermediate powder, which is then granulated and sintered to obtain manganese-zinc power ferrite material.

[0024] The main components include Fe2O3, ZnO and MnO;

[0025] The first additive is SnO2 and Co2O3, and the second additive is CaCO3 and ZrO2.

[0026] In this invention, SnO2 and Co2O3 are first mixed with the main components. Since both act within the crystal lattice, their combined action refines the particle size and participates in the solid-state reaction during pre-sintering, making them easier to penetrate the crystal lattice. Furthermore, considering that some SnO2 that does not enter the crystal lattice may segregate at the grain boundary layer, and given its melting point of 1127°C, it will form a liquid phase during sintering, leading to rapid grain growth and increased porosity. Compared to adding SnO2 in step (2), adding SnO2 in step (1) has the advantage of reducing SnO2 segregation at the grain boundary layer, weakening the solid-state reaction, and thus reducing porosity.

[0027] By combining the preparation process with the coordination and content control of various additives in the manganese-zinc power ferrite material, and by combining the raw material ratio of the main components, we can achieve low overall loss in an ultra-wide temperature range of 25-160℃, especially at the high temperature of 160℃, where it still has the effect of low loss.

[0028] As a preferred technical solution of the present invention, the mixing in step (1) includes sand milling.

[0029] Preferably, the grinding time is 1 to 2 hours, such as 1 hour, 1.2 hours, 1.5 hours, 1.8 hours, or 2 hours.

[0030] Preferably, after mixing in step (1) and before pre-firing, drying is also included.

[0031] As a preferred technical solution of the present invention, the pre-firing temperature in step (1) is 750-850°C, for example 750°C, 780°C, 800°C, 820°C or 850°C.

[0032] In this invention, a pre-calcination temperature of 750–850°C can improve the chemical activity of the powder, that is, it is easier to carry out solid-phase reaction during sintering, which is beneficial to improving the various properties of manganese-zinc power ferrite materials. However, a higher pre-calcination temperature will cause uneven particle size distribution of the powder, and discontinuous crystal growth may occur during sintering, which will reduce the performance of the ferrite material. In addition, in order to maintain a uniform particle size of the pre-calcined powder and facilitate subsequent mixing, grinding is required. A higher pre-calcination temperature will also increase the grinding time of the pre-calcined powder.

[0033] Preferably, the heat preservation time for preheating in step (1) is 2 to 4 hours, such as 2 hours, 2.5 hours, 3 hours, 3.5 hours or 4 hours.

[0034] As a preferred technical solution of the present invention, the mixing in step (2) includes sand milling.

[0035] Preferably, the grinding time is 2 to 4 hours, for example, 2, 2.5 hours, 3 hours, 3.5 hours or 4 hours.

[0036] As a preferred technical solution of the present invention, after mixing in step (2) and before granulation, drying is also included.

[0037] Preferably, the median particle size D50 of the dried powder is 0.9 to 1.2 μm, for example, 0.9 μm, 1.0 μm, 1.1 μm or 1.2 μm.

[0038] Preferably, the granulating agent used in step (2) includes polyvinyl alcohol and / or polyvinyl butyral.

[0039] Preferably, based on the mass of the intermediate powder, the amount of granulating agent added is 5 to 10 wt%, for example, 5 wt%, 6 wt%, 7 wt%, 8 wt%, 9 wt%, or 10 wt%.

[0040] As a preferred technical solution of the present invention, the sintering temperature in step (2) is 1260-1300℃, for example 1260℃, 1270℃, 1280℃, 1290℃ or 1300℃.

[0041] Preferably, the holding time for sintering in step (2) is 150 to 250 minutes, such as 150 minutes, 180 minutes, 200 minutes, 230 minutes or 250 minutes.

[0042] As a preferred technical solution of the present invention, the preparation method includes the following steps:

[0043] (1) Mix the main components, SnO2 and Co2O3 for 1-2 hours, dry them, and then pre-calcine them at 750-850℃ for 2-4 hours to obtain the pre-calcined material;

[0044] The main components include Fe2O3, ZnO and MnO;

[0045] (2) The pre-burned material described in step (1) is mixed with CaCO3 and ZrO2 for 2-4 hours and dried to obtain intermediate powder with a median particle size D50 of 0.9-1.2 μm. Based on the mass of the intermediate powder, 5-10 wt% of granulating agent is added for granulation, and sintered at 1260-1300℃ for 150-250 min to obtain manganese-zinc power ferrite material.

[0046] The mixing process includes sand milling; the granulating agent used in the granulation process includes polyvinyl alcohol and / or polyvinyl butyral.

[0047] Compared with the prior art, the present invention has at least the following beneficial effects:

[0048] 1) The manganese-zinc power ferrite material described in this invention has a power consumption of ≤360kW / m at 25℃ under the conditions of 100kHz and 200mT within a temperature range of 25~160℃. 3 Power consumption at 100℃ ≤ 310kW / m 3 Power consumption at 160℃ ≤360kW / m 3 Especially at high temperatures of 160℃, the power consumption remains low;

[0049] 2) This invention mixes the additives in stages, ensuring that the additives acting on the crystal lattice can more easily enter the interior of the crystal lattice and interact with Fe. 2+ This creates a synergistic effect and reduces the segregation of SnO2 at the grain boundary layer, weakening the solid-phase reaction and thus reducing porosity.

[0050] 3) The preparation process of this invention is simple and low in cost, and the manganese-zinc power ferrite material prepared has wide temperature range and low loss characteristics. Detailed Implementation

[0051] To facilitate understanding of the present invention, the following embodiments are provided. Those skilled in the art should understand that these embodiments are merely illustrative and should not be construed as limiting the scope of the invention.

[0052] Unless otherwise stated, the raw materials and reagents used in the following examples are commercially available products or can be prepared by known methods.

[0053] Example 1

[0054] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The main components of the manganese-zinc power ferrite material include 69.60 wt% Fe2O3, 6.0 wt% ZnO and 24.4 wt% MnO, and the additives consist of 1500 ppm SnO2, 1000 ppm CaCO3, 200 ppm ZrO2 and 4000 ppm Co2O3.

[0055] The preparation method includes the following steps:

[0056] (1) Weigh the main components according to the formula: 69.60wt% Fe2O3, 6.0wt% ZnO and 24.4wt% MnO (the total mass of the main components is 100%), and the additives: 1500ppm SnO2, 1000ppm CaCO3, 200ppm ZrO2 and 4000ppm Co2O3 (all based on the total mass of the main components).

[0057] The main components Fe2O3, ZnO and MnO, and additives SnO2 and Co2O3 were mixed and milled for 1 hour. The mass ratio of the total mass of raw materials, milling balls and water was 1:6:1.5. After drying, the mixture was pre-calcined at 800°C for 3 hours in an air atmosphere to obtain pre-calcined material.

[0058] (2) The obtained pre-burned material, CaCO3 and ZrO2 were mixed and milled for 3 hours. The mass ratio of the total mass of raw materials, grinding balls and water was 1:6:1.5. After drying, intermediate powder with a median particle size D50 of 1 μm was obtained. Then, based on the mass of the intermediate powder, 8 wt% PVA was added for granulation and molding. The mixture was sintered at 1280℃ for 180 min to obtain the manganese-zinc power ferrite material.

[0059] Example 2

[0060] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The main components of the manganese-zinc power ferrite material include 69.68 wt% Fe2O3, 5.5 wt% ZnO and 24.82 wt% MnO, and the additives consist of 1200 ppm SnO2, 800 ppm CaCO3, 300 ppm ZrO2 and 3500 ppm Co2O3.

[0061] The preparation method includes the following steps:

[0062] (1) Weigh the main components according to the formula: 69.68wt% Fe2O3, 5.5wt% ZnO and 24.82wt% MnO (the total mass of the main components is 100%), and the additives: 1200ppm SnO2, 800ppm CaCO3, 300ppm ZrO2 and 3500ppm Co2O3 (all based on the total mass of the main components).

[0063] The main components Fe2O3, ZnO and MnO, and additives SnO2 and Co2O3 were mixed and milled for 2 hours. The mass ratio of the total mass of raw materials, milling balls and water was 1:6:1.5. After drying, the mixture was pre-calcined at 750°C for 4 hours in an air atmosphere to obtain pre-calcined material.

[0064] (2) The obtained pre-burned material, CaCO3 and ZrO2 were mixed and milled for 3 hours. The mass ratio of the total mass of raw materials, grinding balls and water was 1:5:2. After drying, intermediate powder with a median particle size D50 of 0.9 μm was obtained. Then, based on the mass of the intermediate powder, 5 wt% PVA was added for granulation and molding. The mixture was sintered at 1260℃ for 180 min to obtain the manganese-zinc power ferrite material.

[0065] Example 3

[0066] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The main components of the manganese-zinc power ferrite material include 69.50 wt% Fe2O3, 6.4 wt% ZnO and 24.1 wt% MnO, and the additives consist of 1800 ppm SnO2, 1200 ppm CaCO3, 400 ppm ZrO2 and 4400 ppm Co2O3.

[0067] The preparation method includes the following steps:

[0068] (1) Weigh the main components according to the formula: 69.50wt% Fe2O3, 6.4wt% ZnO and 24.1wt% MnO (the total mass of the main components is 100%), and the additives: 1800ppm SnO2, 1200ppm CaCO3, 400ppm ZrO2 and 4400ppm Co2O3 (all based on the total mass of the main components).

[0069] The main components Fe2O3, ZnO and MnO, and additives SnO2 and Co2O3 were mixed and milled for 2 hours. The mass ratio of the total mass of the raw materials, the milling balls and water was 1:7:1. After drying, the mixture was pre-calcined at 850°C for 2 hours in an air atmosphere to obtain the pre-calcined material.

[0070] (2) The obtained pre-burned material, CaCO3 and ZrO2 were mixed and milled for 2 hours. The mass ratio of the total mass of the raw materials, the milling balls and water was 1:7:1. After drying, intermediate powder with a median particle size D50 of 1.2 μm was obtained. Then, based on the mass of the intermediate powder, 10 wt% PVA was added for granulation and molding. The mixture was sintered at 1280℃ for 150 min to obtain the manganese-zinc power ferrite material.

[0071] Example 4

[0072] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that the amount of SnO2 added is 500 ppm, while the remaining components and contents are the same as in Embodiment 1.

[0073] In the preparation method described above, the amount of SnO2 added is adjusted to 500 ppm, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0074] Example 5

[0075] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that the amount of SnO2 added is 2500 ppm, while the remaining components and contents are the same as in Embodiment 1.

[0076] In the preparation method described above, the amount of SnO2 added is adjusted to 2500 ppm, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0077] Example 6

[0078] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that the amount of CaCO3 added is 300 ppm, while the remaining components and contents are the same as in Embodiment 1.

[0079] In the preparation method described above, the amount of CaCO3 added is adjusted to 300 ppm, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0080] Example 7

[0081] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that the amount of CaCO3 added is 1500 ppm, while the remaining components and contents are the same as in Embodiment 1.

[0082] In the preparation method described above, the amount of CaCO3 added is adjusted to 1500 ppm, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0083] Example 8

[0084] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that the amount of ZrO2 added is 50 ppm, while the remaining components and contents are the same as in Embodiment 1.

[0085] In the preparation method described above, the amount of ZrO2 added is adjusted to 50 ppm, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0086] Example 9

[0087] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that the amount of ZrO2 added is 600 ppm, while the remaining components and contents are the same as in Embodiment 1.

[0088] In the preparation method described above, the amount of ZrO2 added is adjusted to 600 ppm, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0089] Example 10

[0090] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that the amount of Co2O3 added is 2000 ppm, while the remaining components and contents are the same as in Embodiment 1.

[0091] In the preparation method described above, the amount of Co2O3 added is adjusted to 2000 ppm, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0092] Example 11

[0093] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that the amount of Co2O3 added is 5000ppm, while the remaining components and contents are the same as in Embodiment 1.

[0094] In the preparation method described above, the amount of Co2O3 added is adjusted to 5000 ppm, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0095] Example 12

[0096] This embodiment provides a manganese-zinc power ferrite material and its preparation method, wherein the composition and content of the manganese-zinc power ferrite material are consistent with those in Example 1;

[0097] The difference between the preparation method described above and Example 1 is that in step (1), SnO2 is first mixed and milled with the main components Fe2O3, ZnO and MnO, and Co2O3 is added in step (2). The rest of the preparation methods and parameters are the same as those in Example 1.

[0098] Example 13

[0099] This embodiment provides a manganese-zinc power ferrite material and its preparation method, wherein the composition and content of the manganese-zinc power ferrite material are consistent with those in Example 1;

[0100] The difference between the preparation method described above and Example 1 is that in step (1), only Co2O3 is first mixed and milled with the main components Fe2O3, ZnO and MnO, and SnO2 is added in step (2). The rest of the preparation methods and parameters are the same as those in Example 1.

[0101] Example 14

[0102] This embodiment provides a manganese-zinc power ferrite material and its preparation method, wherein the composition and content of the manganese-zinc power ferrite material are consistent with those in Example 1;

[0103] The difference between the preparation method described above and Example 1 is that in step (1), the main components Fe2O3, ZnO and MnO are mixed first, and SnO2 and Co2O3 are added in step (2). The remaining preparation methods and parameters are consistent with those of Example 1.

[0104] Example 15

[0105] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that, based on the mass of the main components as 100%, the mass percentage of Fe2O3 is 69.30 wt%, the mass percentage of MnO is 24.7 wt%, and the remaining components and contents are consistent with those in Embodiment 1.

[0106] In the preparation method described above, the mass percentage of Fe2O3 is adjusted to 69.30 wt%, the mass percentage of MnO is adjusted to 24.7 wt%, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0107] Example 16

[0108] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that, based on the mass of the main components as 100%, the mass percentage of Fe2O3 is 69.90 wt%, the mass percentage of MnO is 24.1 wt%, and the remaining components and contents are consistent with those in Embodiment 1.

[0109] In the preparation method described above, the mass percentage of Fe2O3 is adjusted to 69.90 wt%, the mass percentage of ZnO is adjusted to 24.1 wt%, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0110] Example 17

[0111] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that, based on the mass of the main components as 100%, the mass percentage of ZnO is 5.2 wt%, the mass percentage of MnO is 25.2 wt%, and the remaining components and contents are consistent with those in Embodiment 1.

[0112] In the preparation method described above, the mass percentage of ZnO is adjusted to 5.2 wt%, the mass percentage of MnO is adjusted to 25.2 wt%, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0113] Example 18

[0114] This embodiment provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and that in Embodiment 1 is that, based on the mass of the main components as 100%, the mass percentage of ZnO is 6.6 wt%, the mass percentage of MnO is 23.8 wt%, and the remaining components and contents are consistent with those in Embodiment 1.

[0115] In the preparation method described above, the mass percentage of ZnO is adjusted to 6.6 wt%, the mass percentage of MnO is adjusted to 23.8 wt%, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0116] Comparative Example 1

[0117] This comparative example provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and Example 1 is that the addition of SnO2 is omitted, while the remaining components and contents are the same as in Example 1.

[0118] In the preparation method described above, the addition of SnO2 is omitted, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0119] Comparative Example 2

[0120] This comparative example provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and Example 1 is that the addition of ZrO2 is omitted, while the remaining components and contents are the same as in Example 1.

[0121] In the preparation method described above, the addition of ZrO2 is omitted, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0122] Comparative Example 3

[0123] This comparative example provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and Example 1 is that the addition of Co2O3 is omitted, while the remaining components and contents are the same as in Example 1.

[0124] In the preparation method described above, the addition of Co2O3 is omitted, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0125] Comparative Example 4

[0126] This comparative example provides a manganese-zinc power ferrite material and its preparation method. The difference between the manganese-zinc power ferrite material and Example 1 is that the addition of CaCO3 is omitted, while the remaining components and contents are the same as in Example 1.

[0127] In the preparation method described above, the addition of CaCO3 is omitted, and the remaining preparation methods and parameters are consistent with those in Example 1.

[0128] The manganese-zinc power ferrite materials (25×15×8mm material standard rings) provided in Examples 1-18 and Comparative Examples 1-4 were placed on a SY8219 test equipment, and their power consumption (kW / m²) was measured under the following test conditions: 100kHz, 200mT, T=25℃, 100℃, and 160℃. 3 For detailed data, please refer to Table 1.

[0129] Table 1

[0130]

[0131]

[0132] The test results show that:

[0133] (1) As can be seen from Examples 1-3, the manganese-zinc power ferrite material of the present invention has a power consumption of ≤360kW / m at 25℃ under the ultra-wide temperature range of 25~160℃, 100kHz, and 200mT conditions. 3 Power consumption at 100℃ ≤ 310kW / m 3 Power consumption at 160℃ ≤360kW / m 3 ;

[0134] (2) As can be seen from Examples 1 and 4-11, by controlling the addition amounts of SnO2, CaCO3, ZrO2 and Co2O3 within the corresponding ranges, the power consumption at various temperatures can be kept low. In particular, it can ensure that the power consumption of the material is still ≤360kW / m at a high temperature of 160℃. 3 ;

[0135] (3) As can be seen from Examples 1 and 12-14, the present invention mixes SnO2 and Co2O3 together with the main components Fe2O3, ZnO and MnO, which can work together to refine the particle size and make the two easier to enter the crystal lattice. If one or both are added in step (2), the power consumption reduction effect at each temperature cannot be achieved.

[0136] (4) As can be seen from Examples 1 and 15-18, by controlling the content of the main component within the corresponding range, the power consumption at various temperatures can be kept low, especially ensuring that the power consumption of the material is still ≤310kW / m at a high temperature of 100℃. 3 Even at a high temperature of 160℃, the power consumption remains ≤360kW / m 3 ;

[0137] (5) As can be seen from Example 1 and Comparative Examples 1-4, the additive of the present invention is composed of SnO2, CaCO3, ZrO2 and Co2O3. The four play a synergistic role at both the grain boundary and the grain interior. Combined with the raw material ratio of the main component, they together achieve low overall loss in an ultra-wide temperature range of 25 to 160°C. Especially at the high temperature of 160°C, it still has the effect of low loss. If any one of the additives is omitted, the effect of reducing power consumption at each temperature cannot be achieved.

[0138] In summary, this invention, through the coordination and content control of various additives, combined with the raw material ratio of the main components, regulates the composition of the manganese-zinc power ferrite material. Furthermore, by incorporating a stepwise mixing and sintering process for the additives, the overall power loss of the manganese-zinc power ferrite material is kept low over an ultra-wide temperature range of 25–160°C. Specifically, at 100kHz and 200mT, the power consumption at 25°C is ≤360kW / m. 3 Power consumption at 100℃ ≤ 310kW / m 3 Power consumption at 160℃ ≤360kW / m 3 .

[0139] The applicant declares that the above description is only a specific embodiment of the present invention, but the protection scope of the present invention is not limited thereto. Those skilled in the art should understand that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention fall within the protection and disclosure scope of the present invention.

Claims

1. A manganese-zinc power ferrite material, characterized in that, The manganese-zinc power ferrite material includes a main component and additives. The main component includes Fe2O3, ZnO and MnO, and the additives are composed of SnO2, CaCO3, ZrO2 and Co2O3. Based on the mass of the main components as 100%, the Fe2O3 mass is 69.50~69.68wt%, the ZnO mass is 5.5~6.4wt%, and the MnO mass is 23.6~25.4wt%. Based on the total mass of the main components, the amount of SnO2 added is 1000~2000ppm, the amount of CaCO3 added is 500~1200ppm, the amount of ZrO2 added is 100~400ppm, and the amount of Co2O3 added is 3000~4500ppm. The manganese-zinc power ferrite material is prepared by the following method, which includes the following steps: (1) Mix the main component and the first additive evenly, and then pre-calcine to obtain the pre-calcined material; (2) The pre-burned material described in step (1) is mixed evenly with the second additive to obtain intermediate powder, which is then granulated and sintered to obtain manganese-zinc power ferrite material. The first additive is SnO2 and Co2O3, and the second additive is CaCO3 and ZrO2.

2. The manganese-zinc power ferrite material according to claim 1, characterized in that, The manganese-zinc power ferrite material has a power consumption of ≤360kW / m at 25℃ under the following conditions: 100kHz, 200mT, and a temperature range of 25~160℃. 3 Power consumption at 100℃ ≤ 310kW / m 3 Power consumption at 160℃ ≤360kW / m 3 .

3. A method for preparing the manganese-zinc power ferrite material according to claim 1 or 2, characterized in that, The preparation method includes the following steps: (1) Mix the main component and the first additive evenly, and then pre-calcine to obtain the pre-calcined material; (2) The pre-burned material described in step (1) is mixed evenly with the second additive to obtain intermediate powder, which is then granulated and sintered to obtain manganese-zinc power ferrite material. The main components include Fe2O3, ZnO and MnO; The first additive is SnO2 and Co2O3, and the second additive is CaCO3 and ZrO2.

4. The preparation method according to claim 3, characterized in that, The mixing in step (1) includes sand milling.

5. The preparation method according to claim 4, characterized in that, The grinding time is 1 to 2 hours.

6. The preparation method according to claim 3, characterized in that, The preheating temperature in step (1) is 750~850℃.

7. The preparation method according to claim 3, characterized in that, The heat preservation time for preheating in step (1) is 2-4 hours.

8. The preparation method according to claim 3, characterized in that, The mixing in step (2) includes sand milling.

9. The preparation method according to claim 8, characterized in that, The grinding time is 2-4 hours.

10. The preparation method according to claim 3, characterized in that, After mixing in step (2) and before granulation, drying is also included.

11. The preparation method according to claim 10, characterized in that, The median particle size D50 of the dried powder is 0.9~1.2μm.

12. The preparation method according to claim 3, characterized in that, The granulating agent used in step (2) includes polyvinyl alcohol and / or polyvinyl butyral.

13. The preparation method according to claim 12, characterized in that, Based on the mass of the intermediate powder, the amount of granulating agent added is 5~10wt%.

14. The preparation method according to claim 3, characterized in that, The sintering temperature in step (2) is 1260~1300℃.

15. The preparation method according to claim 3, characterized in that, The holding time for sintering in step (2) is 150~250 min.

16. The preparation method according to claim 3, characterized in that, The preparation method includes the following steps: (1) Mix the main components, SnO2 and Co2O3 for 1-2 hours, dry them, and then pre-calcine them at 750-850℃ for 2-4 hours to obtain the pre-calcined material; The main components include Fe2O3, ZnO and MnO; (2) The pre-burned material described in step (1) is mixed with CaCO3 and ZrO2 for 2-4 hours and dried to obtain intermediate powder with a median particle size D50 of 0.9-1.2 μm. Based on the mass of the intermediate powder, 5-10 wt% of granulating agent is added for granulation, and sintered at 1260-1300℃ for 150-250 min to obtain manganese-zinc power ferrite material; The mixing process includes sand milling; the granulating agent used in the granulation process includes polyvinyl alcohol and / or polyvinyl butyral.

17. An application of a manganese-zinc power ferrite material, characterized in that, The manganese-zinc power ferrite material according to claim 1 or 2, or the manganese-zinc power ferrite material prepared by the preparation method according to any one of claims 3-16, is applied to automotive electronic modules.

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