Manganese-zinc ferrite material, its preparation method and application

Abstract

The application provides a manganese-zinc ferrite material and a preparation method and application thereof. The manganese-zinc ferrite material can have an initial permeability μi of 1837 H / m or higher, a saturation magnetic induction intensity Bs of 572 mT or higher at 25 DEG C, and a saturation magnetic induction intensity Bs of 487 mT or higher at 100 DEG C through specific setting of a formula, so that the power conversion efficiency of an electronic component is improved.

Description

Technical Field

[0001] This invention belongs to the technical field of soft magnetic ferrite materials, and relates to a soft magnetic ferrite material, its preparation method and application, and particularly to a manganese zinc ferrite material, its preparation method and application. Background Technology

[0002] To meet the development requirements of power electronic devices, the properties of ferrite materials need further improvement. First, to adapt to the miniaturization requirements of electronic products, ferrite materials must have a high saturation magnetic flux density Bs. Second, to effectively reduce losses introduced by the coil, ferrite materials need a high permeability μi. Third, to reduce the impact of temperature changes in the operating environment and ensure stable electromagnetic performance of the device, ferrite materials also need good temperature stability. Therefore, manganese-zinc ferrite materials need to possess high permeability, high saturation magnetic flux density, and good stability, but achieving a good balance among these three aspects is difficult.

[0003] CN101620908A discloses a manganese-zinc ferrite material with ultra-high saturation magnetic flux density and its preparation method. By limiting the iron oxide content to 63mol%-67mol%, the zinc oxide content to 11mol%-16mol%, and the auxiliary components CaCO3, SiO2, Nb2O5, ZrO2 and NiO, an ultra-high Bs of over 500mT is achieved at a high temperature of 100℃. However, the overall permeability of the manganese-zinc ferrite material under this formulation system is only 800H / m.

[0004] CN117024158A discloses a high-Bs ferrite material and its preparation method. By limiting the iron oxide content to 65mol%-66mol%, the nickel oxide content to 15.5mol%-16.5mol%, and the copper oxide content to 4mol%-5mol%, a saturation magnetic flux density of 488mT at 25℃ is achieved. However, the above formula has a large amount of NiO added, which increases the production cost of the ferrite material.

[0005] CN110171964A discloses a high-Bs, high-strength manganese-zinc ferrite material and its preparation method. By limiting the iron oxide content to 57.5 mol%-62.5 mol%, the zinc oxide content to 11 mol%-14 mol%, and the auxiliary components CaCO3, SiO2, MoO3, ZrO2, V2O5, and SnO, a Bs of 596 mT is achieved at 25℃ and a Bs of 490 mT at 100℃. However, there is room for further improvement in its Bs and temperature stability.

[0006] Therefore, in order to obtain manganese-zinc ferrite materials with high initial permeability, high saturation magnetic induction and low cost, it is necessary to provide a manganese-zinc ferrite material, its preparation method and application. Summary of the Invention

[0007] To address the shortcomings of existing technologies, the present invention aims to provide a manganese-zinc ferrite material, its preparation method, and its application. Through specific formulation settings, the manganese-zinc ferrite material can achieve an initial permeability μi of 1837 H / m or higher, a saturation magnetic induction intensity Bs of 572 mT or higher at 25°C, and a saturation magnetic induction intensity Bs of 487 mT or higher at 100°C, thereby improving the power conversion efficiency of electronic components.

[0008] To achieve this objective, the present invention adopts the following technical solution:

[0009] In a first aspect, the present invention provides a manganese-zinc ferrite material, the manganese-zinc ferrite material comprising a main component and an auxiliary component;

[0010] The raw materials for preparing the main component, in molar percentage, include 62-66 mol% Fe2O3, 14-17 mol% ZnO, and the balance Mn3O4.

[0011] The auxiliary ingredients, based on their mass as a percentage of the main components, include 8000-9000 ppm NiO, 200-800 ppm CaCO3, 300-900 ppm MoO3, 100-300 ppm ZrO2, 200-500 ppm Nb2O5, and 100-500 ppm V2O5.

[0012] The manganese-zinc ferrite material provided by this invention, through specific formulation settings, can achieve an initial magnetic permeability μi of over 2000 H / m, a saturation magnetic induction intensity Bs of over 610 mT at 25°C, and a saturation magnetic induction intensity Bs of over 500 mT at 100°C, thereby improving the power conversion efficiency of electronic components.

[0013] The appropriate amount of Fe2O3 content enables the generated appropriate amount of Fe3O4 to provide positive λs compensation, and the addition of an appropriate amount of Zn ions can dilute the coupling effect of magnetic ions, thereby effectively improving the μi value. In this invention, the molar percentage of Fe2O3 in the raw materials for preparing the main component is 62-66 mol%, for example, it can be 62 mol%, 63 mol%, 64 mol%, 65 mol%, or 66 mol%, but is not limited to the listed values. Other values ​​not listed within the numerical range are also applicable, preferably 63-64 mol%. In this invention, the molar percentage of ZnO in the raw materials for preparing the main component is 14-17 mol%, for example, it can be 14 mol%, 15 mol%, 16 mol%, or 17 mol%, but is not limited to the listed values. Other values ​​not listed within the numerical range are also applicable, preferably 16-17 mol%.

[0014] In the preparation of auxiliary components, the addition of an appropriate amount of NiO can increase the permeability between magnetic ions. 2- The increased number of superexchange pairs and the higher Curie temperature of the generated NiFe2O4 compared to FeFe2O4 improve the temperature stability of Bs. Furthermore, the iron-rich formulation of the main component releases a significant amount of oxygen during preparation, leading to porosity in the manganese-zinc ferrite material and reducing its sintering density. This invention addresses this by adding an appropriate amount of MoO3. The MnMoO4 formed at the grain boundaries during sintering hinders the growth of MnZn ferrite grains. This hindrance facilitates the expulsion of oxygen generated during Fe2O3 reduction, thus ensuring the sintering density of the manganese-zinc ferrite material. Simultaneously, the addition of Nb2O5 promotes grain growth, increasing the material's density and initial permeability. The combined addition of both produces a synergistic effect, further enhancing the material's performance.

[0015] In this invention, the NiO in the auxiliary component accounts for 8000-9000 ppm of the main component mass, for example, it can be 8000 ppm, 8200 ppm, 8500 ppm, 8800 ppm or 9000 ppm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable, preferably 8800-9000 ppm.

[0016] In this invention, the CaCO3 in the auxiliary component accounts for 200-800 ppm of the main component mass, for example, it can be 200 ppm, 300 ppm, 400 ppm, 500 ppm, 600 ppm, 700 ppm or 800 ppm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable, preferably 300-500.

[0017] In this invention, the MoO3 in the auxiliary component accounts for 300-900 ppm of the main component mass, for example, it can be 300 ppm, 400 ppm, 500 ppm, 600 ppm, 700 ppm, 800 ppm or 900 ppm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable, preferably 300-400 ppm.

[0018] In this invention, the ZrO2 in the auxiliary component accounts for 100-300 ppm of the main component mass, for example, it can be 100 ppm, 150 ppm, 200 ppm, 250 ppm or 300 ppm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable, preferably 100-200 ppm.

[0019] In this invention, the Nb2O5 in the auxiliary component accounts for 200-500 ppm of the main component mass, for example, it can be 200 ppm, 300 ppm, 400 ppm or 500 ppm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable, preferably 200-300 ppm.

[0020] In this invention, the V2O5 in the auxiliary components accounts for 100-500 ppm of the main component mass, for example, it can be 100 ppm, 200 ppm, 300 ppm, 400 ppm or 500 ppm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable, preferably 250-300 ppm of V2O5.

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

[0022] (1) Mix the main components of the raw materials according to the formula, and then perform pre-calcination treatment to obtain pre-calcined material;

[0023] (2) Mix the auxiliary ingredients with the pre-calcined material obtained in step (1) according to the formula amount, crush them, and obtain powder;

[0024] (3) The powder obtained in step (2) is granulated, shaped and sintered to obtain the manganese zinc ferrite material.

[0025] With the specific formulation provided by the manganese-zinc ferrite material in the first aspect of the present invention, and with the aid of a suitable preparation method, it is possible to prepare a manganese-zinc ferrite material that has both high initial permeability, high saturation magnetic induction intensity and low production cost.

[0026] Preferably, the heating rate of the pre-calcination treatment in step (1) is 2-5℃ / min, for example, it can be 2℃ / min, 3℃ / min, 4℃ / min or 5℃ / min, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0027] Preferably, the temperature of the pre-firing treatment in step (1) is 800-850℃, for example, it can be 800℃, 810℃, 820℃, 840℃ or 850℃, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0028] Preferably, the heat preservation time of the pre-firing treatment in step (1) is 2-4 hours, for example, it can be 2 hours, 2.5 hours, 3 hours, 3.5 hours or 4 hours, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0029] Preferably, the pre-firing treatment described in step (1) is followed by air cooling.

[0030] Preferably, the oxygen content during sintering in step (3) is controlled to be 1-21 vol%, for example, it can be 1 vol%, 3 vol%, 5 vol%, 6 vol%, 9 vol%, 10 vol%, 15 vol%, 20 vol%, or 21 vol%, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0031] Preferably, the sintering temperature in step (3) is 1350-1450℃, for example, it can be 1350℃, 1380℃, 1400℃, 1420℃ or 1450℃, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0032] Preferably, the sintering in step (3) includes a first sintering and a second sintering performed sequentially.

[0033] Preferably, the oxygen content is controlled to be 19-21 vol% during the first sintering, for example, it can be 19 vol%, 20 vol%, or 21 vol%, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0034] Preferably, the first sintering temperature is 1350-1400℃, for example, it can be 1350℃, 1360℃, 1380℃, 1390℃ or 1400℃, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0035] Preferably, the first sintering time is 5-8 hours, for example, it can be 5 hours, 6 hours, 7 hours or 8 hours, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0036] Preferably, the oxygen content is controlled to be 1-5 vol% during the second sintering process, for example, it can be 1 vol%, 3 vol%, 4 vol%, or 5 vol%, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0037] Preferably, the second sintering temperature is 1350-1400℃, for example, it can be 1350℃, 1360℃, 1380℃, 1390℃ or 1400℃, but is not limited to the listed values, and other unlisted values ​​within the range are also applicable.

[0038] Preferably, the second sintering time is 1-2 hours, for example, it can be 1 hour, 1.5 hours or 2 hours, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0039] Preferably, the cooling after sintering is carried out under conditions of balanced oxygen partial pressure.

[0040] Preferably, the mixing method in step (1) includes wet ball milling.

[0041] Preferably, the wet ball milling is carried out in a planetary ball mill with a frequency of 40-60Hz, such as 40Hz, 45Hz, 50Hz, 55Hz or 60Hz, but not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0042] Preferably, the wet ball milling is carried out in a planetary ball mill with a rotational speed of 200-300 r / min, for example, 200 r / min, 250 r / min or 300 r / min, but not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0043] Preferably, the mixing method in step (2) includes wet sand milling.

[0044] Preferably, the wet sand milling is carried out in a planetary ball mill with a frequency of 40-60Hz, such as 40Hz, 45Hz, 50Hz, 55Hz or 60Hz, but not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0045] Preferably, the wet sand milling is carried out in a planetary ball mill with a rotational speed of 200-300 r / min, for example, 200 r / min, 250 r / min or 300 r / min, but not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0046] Preferably, the particle size X50 of the powder in step (2) is 1.3-1.55μm, for example, it can be 1.3μm, 1.35μm, 1.4μm, 1.42μm, 1.45μm, 1.5μm or 1.55μm, but is not limited to the listed values. Other unlisted values ​​within the range are also applicable.

[0047] As a preferred embodiment of the preparation method provided in the second aspect of the present invention, the preparation method includes the following steps:

[0048] (1) Mix the main components of the raw materials by wet ball milling for 20-60 min according to the formula, then heat the mixture to 800-850℃ at a heating rate of 2-5℃ / min for 2-4 h for pre-calcination, and air cool to obtain the pre-calcined material.

[0049] Wet ball milling is carried out in a planetary ball mill with a frequency of 40-60Hz and a rotation speed of 200-300r / min.

[0050] (2) Mix the auxiliary components with the pre-burned material obtained in step (1) by wet sand milling according to the formula amount, and crush to obtain powder with a particle size X50 of 1.3-1.55μm;

[0051] Wet sand milling is carried out in a planetary ball mill with a frequency of 40-60Hz and a rotation speed of 200-300r / min.

[0052] (3) The powder obtained in step (2) is granulated, shaped and sintered to obtain the manganese zinc ferrite material;

[0053] The sintering includes a first sintering and a second sintering performed sequentially.

[0054] During the first sintering process, the oxygen content is controlled at 19-21 vol%, the temperature is 1350-1400℃, and the time is 5-8 hours.

[0055] During the second sintering process, the oxygen content is controlled at 1-5 vol%, the temperature is 1350-1400℃, and the time is 1-2 hours.

[0056] Thirdly, the present invention provides an application of the manganese-zinc ferrite material described in the second aspect, characterized in that the manganese-zinc ferrite material is used in electronic components.

[0057] The numerical range described in this invention includes not only the point values ​​listed above, but also any point values ​​within the numerical ranges not listed above. Due to space limitations and for the sake of brevity, this invention will not exhaustively list all the specific point values ​​included in the range.

[0058] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0059] The manganese-zinc ferrite material provided by this invention, through specific formulation settings, can achieve an initial permeability μi of 1837 H / m or higher, a saturation magnetic induction intensity Bs of 572 mT or higher at 25°C, and a saturation magnetic induction intensity Bs of 487 mT or higher at 100°C; preferably, it can achieve an initial permeability μi of 2000 H / m or higher, a saturation magnetic induction intensity Bs of 610 mT or higher at 25°C, and a saturation magnetic induction intensity Bs of 500 mT or higher at 100°C, thereby improving the power conversion efficiency of electronic components. Detailed Implementation

[0060] The technical solution of the present invention will be further illustrated below through specific embodiments.

[0061] Example 1

[0062] This embodiment provides a manganese-zinc ferrite material, which includes a main component and auxiliary components, the composition of which is shown in Table 1.

[0063] The preparation method of the manganese-zinc ferrite material provided in this embodiment includes the following steps:

[0064] (1) Mix the main components of the raw materials by wet ball milling for 30 min according to the formula, and then heat them to 850℃ at a heating rate of 5℃ / min for 3 h for pre-calcination treatment, and air-cool them to obtain the pre-calcined material.

[0065] Wet ball milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 250 r / min.

[0066] (2) Mix the auxiliary components with the pre-burned material obtained in step (1) by wet sand milling according to the formula amount, and crush to obtain powder with a particle size X50 of 1.41μm;

[0067] Wet sand milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 250 r / min.

[0068] (3) The powder obtained in step (2) is mixed with 10 wt% of conventional PVA (polyvinyl alcohol) by powder mass, and then sprayed and granulated, and granulated through a 30-mesh sieve to obtain granulated material; the granulated material is pressed into a green body with a diameter of φ25mm×φ15mm×8mm; then the green body is sintered and cooled under balanced oxygen partial pressure to obtain the manganese zinc ferrite material;

[0069] The sintering includes a first sintering and a second sintering performed sequentially, during which the oxygen content is controlled using N2.

[0070] During the first sintering process, the oxygen content was controlled at 21 vol%, the temperature was 1350℃, and the time was 5 hours.

[0071] During the second sintering process, the oxygen content is controlled at 3 vol%, the temperature is 1350℃, and the time is 1 hour.

[0072] Example 2

[0073] This embodiment provides a manganese-zinc ferrite material, which includes a main component and auxiliary components, the composition of which is shown in Table 1.

[0074] The preparation method of the manganese-zinc ferrite material provided in this embodiment includes the following steps:

[0075] (1) Mix the main components of the raw materials by wet ball milling for 30 min according to the formula, and then heat them to 850℃ at a heating rate of 5℃ / min for 3 h for pre-calcination treatment, and air-cool them to obtain the pre-calcined material.

[0076] Wet ball milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 250 r / min.

[0077] (2) Mix the auxiliary components with the pre-burned material obtained in step (1) by wet sand milling according to the formula amount, and crush to obtain powder with a particle size X50 of 1.33μm;

[0078] Wet sand milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 270 r / min.

[0079] (3) The powder obtained in step (2) is mixed with 10 wt% of conventional PVA (polyvinyl alcohol) by powder mass, and then sprayed and granulated, and granulated through a 30-mesh sieve to obtain granulated material; the granulated material is pressed into a green body with a diameter of φ25mm×φ15mm×8mm; then the green body is sintered and cooled under balanced oxygen partial pressure to obtain the manganese zinc ferrite material;

[0080] The sintering includes a first sintering and a second sintering performed sequentially, during which the oxygen content is controlled using N2.

[0081] During the first sintering process, the oxygen content was controlled at 21 vol%, the temperature was 1370℃, and the time was 5 hours.

[0082] During the second sintering process, the oxygen content was controlled at 3 vol%, the temperature was 1370℃, and the time was 1 hour.

[0083] Example 3

[0084] This embodiment provides a manganese-zinc ferrite material, which includes a main component and auxiliary components, the composition of which is shown in Table 1.

[0085] The preparation method of the manganese-zinc ferrite material provided in this embodiment includes the following steps:

[0086] (1) Mix the main components of the raw materials by wet ball milling for 30 min according to the formula, and then heat them to 850℃ at a heating rate of 5℃ / min for 3 h for pre-calcination treatment, and air-cool them to obtain the pre-calcined material.

[0087] Wet ball milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 250 r / min.

[0088] (2) Mix the auxiliary components with the pre-burned material obtained in step (1) by wet sand milling according to the formula amount, and crush to obtain powder with a particle size X50 of 1.30μm;

[0089] Wet sand milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 250 r / min.

[0090] (3) The powder obtained in step (2) is mixed with 10 wt% of conventional PVA (polyvinyl alcohol) by powder mass, and then sprayed and granulated, and granulated through a 30-mesh sieve to obtain granulated material; the granulated material is pressed into a green body with a diameter of φ25mm×φ15mm×8mm; then the green body is sintered and cooled under balanced oxygen partial pressure to obtain the manganese zinc ferrite material;

[0091] The sintering includes a first sintering and a second sintering performed sequentially, during which the oxygen content is controlled using N2.

[0092] During the first sintering process, the oxygen content was controlled at 21 vol%, the temperature at 1365℃, and the time at 6 hours.

[0093] During the second sintering process, the oxygen content was controlled at 3 vol%, the temperature was 1365℃, and the time was 2 hours.

[0094] Example 4

[0095] This embodiment provides a manganese-zinc ferrite material, which includes a main component and auxiliary components, the composition of which is shown in Table 1.

[0096] The preparation method of the manganese-zinc ferrite material provided in this embodiment includes the following steps:

[0097] (1) Mix the main components of the raw materials by wet ball milling for 30 min according to the formula, and then heat them to 850℃ at a heating rate of 5℃ / min for 3 h for pre-calcination treatment, and air-cool them to obtain the pre-calcined material.

[0098] Wet ball milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 250 r / min.

[0099] (2) Mix the auxiliary components with the pre-burned material obtained in step (1) by wet sand milling according to the formula amount, and crush to obtain powder with a particle size X50 of 1.42μm;

[0100] Wet sand milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 250 r / min.

[0101] (3) The powder obtained in step (2) is mixed with 10 wt% of conventional PVA (polyvinyl alcohol) by powder mass, and then sprayed and granulated, and granulated through a 30-mesh sieve to obtain granulated material; the granulated material is pressed into a green body with a diameter of φ25mm×φ15mm×8mm; then the green body is sintered and cooled under balanced oxygen partial pressure to obtain the manganese zinc ferrite material;

[0102] The sintering includes a first sintering and a second sintering performed sequentially, during which the oxygen content is controlled using N2.

[0103] During the first sintering process, the oxygen content was controlled at 21 vol%, the temperature at 1365℃, and the time at 6 hours.

[0104] During the second sintering process, the oxygen content was controlled at 1.5 vol%, the temperature at 1365℃, and the time at 2 hours.

[0105] Example 5

[0106] This embodiment provides a manganese-zinc ferrite material, which includes a main component and auxiliary components, the composition of which is shown in Table 1.

[0107] The preparation method of the manganese-zinc ferrite material provided in this embodiment includes the following steps:

[0108] (1) Mix the main components of the raw materials by wet ball milling for 30 min according to the formula, and then heat them to 800℃ at a heating rate of 5℃ / min for 3 h for pre-calcination treatment, and air-cool them to obtain the pre-calcined material.

[0109] Wet ball milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 250 r / min.

[0110] (2) Mix the auxiliary components with the pre-burned material obtained in step (1) by wet sand milling according to the formula amount, and crush to obtain powder with a particle size X50 of 1.38μm;

[0111] Wet sand milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 260 r / min.

[0112] (3) The powder obtained in step (2) is mixed with 10 wt% of conventional PVA (polyvinyl alcohol) by powder mass, and then sprayed and granulated, and granulated through a 30-mesh sieve to obtain granulated material; the granulated material is pressed into a green body with a diameter of φ25mm×φ15mm×8mm; then the green body is sintered and cooled under balanced oxygen partial pressure to obtain the manganese zinc ferrite material;

[0113] The sintering includes a first sintering and a second sintering performed sequentially, during which the oxygen content is controlled using N2.

[0114] During the first sintering process, the oxygen content was controlled at 21 vol%, the temperature at 1365℃, and the time at 6 hours.

[0115] During the second sintering process, the oxygen content was controlled at 1.5 vol%, the temperature at 1365℃, and the time at 2 hours.

[0116] Example 6

[0117] This embodiment provides a manganese-zinc ferrite material, which includes a main component and auxiliary components, the composition of which is shown in Table 1.

[0118] The preparation method of the manganese-zinc ferrite material provided in this embodiment includes the following steps:

[0119] (1) Mix the main components of the raw materials by wet ball milling for 30 min according to the formula, and then heat them to 850℃ at a heating rate of 5℃ / min for 3 h for pre-calcination treatment, and air-cool them to obtain the pre-calcined material.

[0120] Wet ball milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 250 r / min.

[0121] (2) Mix the auxiliary components with the pre-burned material obtained in step (1) by wet sand milling according to the formula amount, and crush to obtain powder with a particle size X50 of 1.34μm;

[0122] Wet sand milling is carried out in a planetary ball mill with a frequency of 50 Hz and a rotation speed of 260 r / min.

[0123] (3) The powder obtained in step (2) is mixed with 10 wt% of conventional PVA (polyvinyl alcohol) by powder mass, and then sprayed and granulated, and granulated through a 30-mesh sieve to obtain granulated material; the granulated material is pressed into a green body with a diameter of φ25mm×φ15mm×8mm; then the green body is sintered and cooled under balanced oxygen partial pressure to obtain the manganese zinc ferrite material;

[0124] The sintering includes a first sintering and a second sintering performed sequentially, during which the oxygen content is controlled using N2.

[0125] During the first sintering process, the oxygen content was controlled at 21 vol%, the temperature was 1350℃, and the time was 5 hours.

[0126] During the second sintering process, the oxygen content is controlled at 1 vol%, the temperature is 1350℃, and the time is 1 hour.

[0127] Example 7

[0128] This embodiment provides a manganese-zinc ferrite material, which includes a main component and an auxiliary component, and the composition of the main component and the auxiliary component is the same as that in Embodiment 4.

[0129] The preparation method of the manganese-zinc ferrite material provided in this embodiment includes the following steps:

[0130] (1) The main components of the raw materials were mixed by wet ball milling for 20 min according to the formula, and then heated to 800℃ at a heating rate of 2℃ / min for 4 h for pre-calcination treatment, followed by air cooling to obtain the pre-calcined material.

[0131] Wet ball milling is carried out in a planetary ball mill with a frequency of 40 Hz and a rotation speed of 200 r / min.

[0132] (2) Mix the auxiliary components with the pre-burned material obtained in step (1) by wet sand milling according to the formula amount, and crush to obtain powder with a particle size X50 of 1.55μm;

[0133] Wet sand milling is carried out in a planetary ball mill with a frequency of 40Hz and a rotation speed of 200r / min.

[0134] (3) The powder obtained in step (2) is mixed with 10 wt% of conventional PVA (polyvinyl alcohol) by powder mass, and then sprayed and granulated, and granulated through a 30-mesh sieve to obtain granulated material; the granulated material is pressed into a green body with a diameter of φ25mm×φ15mm×8mm; then the green body is sintered and cooled under balanced oxygen partial pressure to obtain the manganese zinc ferrite material;

[0135] The sintering includes a first sintering and a second sintering performed sequentially, during which the oxygen content is controlled using N2.

[0136] During the first sintering process, the oxygen content was controlled at 19 vol%, the temperature was 1400℃, and the time was 8 hours.

[0137] During the second sintering process, the oxygen content is controlled at 5 vol%, the temperature is 1400℃, and the time is 1 hour.

[0138] Example 8

[0139] This embodiment provides a manganese-zinc ferrite material, which includes a main component and an auxiliary component, and the composition of the main component and the auxiliary component is the same as that in Embodiment 4.

[0140] The preparation method of the manganese-zinc ferrite material provided in this embodiment includes the following steps:

[0141] (1) The main components of the raw materials were mixed by wet ball milling for 60 min according to the formula, and then pre-calcined at 850°C for 2 h at a heating rate of 5°C / min. The pre-calcined material was obtained by air cooling.

[0142] Wet ball milling is carried out in a planetary ball mill with a frequency of 60 Hz and a rotation speed of 300 r / min.

[0143] (2) Mix the auxiliary components with the pre-burned material obtained in step (1) by wet sand milling according to the formula amount, and crush to obtain powder with a particle size X50 of 1.37μm;

[0144] Wet sand milling is carried out in a planetary ball mill with a frequency of 60 Hz and a rotation speed of 300 r / min.

[0145] (3) The powder obtained in step (2) is mixed with 10 wt% of conventional PVA (polyvinyl alcohol) by powder mass, and then sprayed and granulated, and granulated through a 30-mesh sieve to obtain granulated material; the granulated material is pressed into a green body with a diameter of φ25mm×φ15mm×8mm; then the green body is sintered and cooled under balanced oxygen partial pressure to obtain the manganese zinc ferrite material;

[0146] The sintering includes a first sintering and a second sintering performed sequentially, during which the oxygen content is controlled using N2.

[0147] During the first sintering process, the oxygen content was controlled at 21 vol%, the temperature was 1350℃, and the time was 5 hours.

[0148] During the second sintering process, the oxygen content is controlled at 1 vol%, the temperature is 1350℃, and the time is 2 hours.

[0149] The difference between Comparative Examples 1-9 and Comparative Examples 9-14 and Example 4 lies in the composition of the manganese-zinc ferrite material. The composition of the main component and auxiliary components is shown in Table 1.

[0150] Table 1

[0151]

[0152] The performance of the manganese-zinc ferrite materials obtained in each embodiment and comparative example was tested, and the results are shown in Table 2:

[0153] Initial permeability μi: Under test conditions of frequency f = 10 kHz and voltage U = 0.25 V, the initial permeability μi was tested using a 10-turn winding method within the room temperature range (25℃ ± 1℃).

[0154] Saturation magnetic flux density Bs: is the magnetic flux density of a magnetic material magnetized to saturation. A DC BH tester was used to test the saturation magnetic induction intensity Bs of the sample. The test conditions were 25℃ and 100℃, Hm was 1194A / m, and N1=N2=20Ts.

[0155] In Table 2, Br refers to the remanent magnetic flux density, and Hc refers to the coercivity.

[0156] Table 2

[0157]

[0158] In summary, the manganese-zinc ferrite material provided by the present invention, through specific formulation settings, can achieve an initial permeability μi of 1837 H / m or higher, a saturation magnetic induction intensity Bs of 572 mT or higher at 25°C, and a saturation magnetic induction intensity Bs of 487 mT or higher at 100°C; preferably, it can achieve an initial permeability μi of 2000 H / m or higher, a saturation magnetic induction intensity Bs of 610 mT or higher at 25°C, and a saturation magnetic induction intensity Bs of 500 mT or higher at 100°C, thereby improving the power conversion efficiency of electronic components.

[0159] The specific embodiments described above further illustrate the purpose, technical solution, and beneficial effects of the present invention. It should be understood that the above descriptions are merely specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A manganese-zinc ferrite material, characterized in that, The manganese-zinc ferrite material includes a main component and auxiliary components; The raw materials for preparing the main component, by molar percentage, include 63.64-66 mol% Fe2O3, 16.51-17 mol% ZnO, and the balance Mn3O4; the raw materials for preparing the auxiliary component, by mass of the main component, include 8000-9000 ppm NiO, 200-800 ppm CaCO3, 300-400 ppm MoO3, 100-300 ppm ZrO2, 200-500 ppm Nb2O5, and 100-500 ppm V2O5.

2. A method for preparing the manganese-zinc ferrite material according to claim 1, characterized in that, The preparation method includes the following steps: (1) Mix the main components of the raw materials according to the formula amount, and then perform pre-calcination treatment to obtain pre-calcined material; (2) Mix the auxiliary ingredients with the pre-calcined material obtained in step (1) according to the formula, crush them, and obtain powder. (3) The powder obtained in step (2) is granulated, shaped and sintered to obtain the manganese zinc ferrite material.

3. The preparation method according to claim 2, characterized in that, The heating rate of the pre-firing treatment in step (1) is 2-5℃ / min.

4. The preparation method according to claim 2, characterized in that, The temperature of the pre-firing treatment in step (1) is 800-850℃.

5. The preparation method according to claim 2, characterized in that, The heat preservation time for the pre-firing treatment in step (1) is 2-4 hours.

6. The preparation method according to claim 2, characterized in that, After the pre-firing treatment described in step (1), the product is air-cooled.

7. The preparation method according to claim 2, characterized in that, In step (3), the oxygen content is controlled to be 1-21 vol during sintering.

8. The preparation method according to claim 2, characterized in that, The sintering temperature in step (3) is 1350-1450℃.

9. The preparation method according to claim 2, characterized in that, The sintering in step (3) includes a first sintering and a second sintering performed sequentially.

10. The preparation method according to claim 9, characterized in that, During the first sintering process, the oxygen content is controlled to be 19-21 vol.

11. The preparation method according to claim 9, characterized in that, The first sintering temperature is 1350-1400℃.

12. The preparation method according to claim 9, characterized in that, The first sintering time is 5-8 hours.

13. The preparation method according to claim 9, characterized in that, During the second sintering process, the oxygen content is controlled to be 1-5 vol.

14. The preparation method according to claim 9, characterized in that, The second sintering temperature is 1350-1400℃.

15. The preparation method according to claim 9, characterized in that, The second sintering time is 1-2 hours.

16. The preparation method according to claim 2, characterized in that, The mixing method in step (1) includes wet ball milling.

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

18. The preparation method according to claim 2, characterized in that, The particle size X50 of the powder in step (2) is 1.3-1.55μm.

19. The preparation method according to claim 2, characterized in that, The preparation method includes the following steps: (1) Mix the main components of the raw materials by wet ball milling for 20-60 min according to the formula, then heat them to 800-850℃ at a heating rate of 2-5℃ / min for 2-4 h for pre-calcination, and air-cool them to obtain the pre-calcined material; Wet ball milling is carried out in a planetary ball mill with a frequency of 40-60Hz and a rotation speed of 200-300r / min. (2) Mix the auxiliary components with the pre-burned material obtained in step (1) by wet sand milling according to the formula amount, and crush to obtain powder with a particle size X50 of 1.3-1.55μm; Wet sand milling is carried out in a planetary ball mill with a frequency of 40-60Hz and a rotation speed of 200-300r / min. (3) The powder obtained in step (2) is granulated, shaped and sintered to obtain the manganese zinc ferrite material; The sintering includes a first sintering and a second sintering performed sequentially. During the first sintering process, the oxygen content is controlled at 19-21 vol%, the temperature is 1350-1400℃, and the time is 5-8 hours. During the second sintering process, the oxygen content is controlled at 1-5 vol%, the temperature is 1350-1400℃, and the time is 1-2 hours.

20. An application of the manganese-zinc ferrite material according to claim 1, characterized in that, The manganese-zinc ferrite material is used in electronic components.

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